Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global #============================================================================== _audit_creation_date '9 March 2005' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' 'Calucci, Lucia' ; Istituto per i Processi Chimico Fisici CNR Area della Ricerca Via G. Moruzzi,1 56124 Pisa Italy ; 'Cloke, F. Geoffrey N.' ; University of Sussex, Falmer Brighton BN19QJ UK ; 'Englert, Ulli' ; Institut fuer Anorganische Chemie RWTH Aachen Prof.-Pirlet-Str.1 52074 Aachen Germany ; 'Hitchcock, Peter B.' ; University of Sussex, Falmer Brighton BN19QJ UK ; 'Pampaloni, Guido' ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento 35 56126 Pisa Italy ; 'Pinzino, Calogero' ; Istituto per i Processi Chimico Fisici CNR Area della Ricerca Via G. Moruzzi,1 56124 Pisa Italy ; 'Puccini, Filippo' ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento 35 56126 Pisa Italy ; 'Volpe, Manuel' ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorgimento 35 56126 Pisa Italy ; #========================================================================== _publ_contact_author_name 'Guido Pampaloni' _publ_contact_author_address ; Dipartimento di Chimica e Chimica Industriale Universita di Pisa Via Risorginmento 35 Pisa I-56126 ITALY ; _publ_contact_author_email PAMPA@DCCI.UNIPI.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis of Chromium(0) and Molybdenum(0) Bis (eta6-arene) Derivatives and Their Monoelectronic Oxidation to [M(eta6-arene)2]+ Cations ; # 4. Text _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXS-97. University of Gottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of Gottingen, Germany. Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, Wisconson, USA. Spek, A. L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; _publ_section_acknowledgements ; Support from the DFG and the Fonds der Chemischen Industrie is gratefully acknowledged. ; _publ_requested_category FM #========================================================================== data_fp4 _database_code_depnum_ccdc_archive 'CCDC 607082' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 O10, C18 H24 Cr' _chemical_formula_sum 'C33 H39 Cr O10' _chemical_formula_weight 647.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr .3209 .6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 19.0585(12) _cell_length_b 20.8529(12) _cell_length_c 31.3141(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12445.0(13) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7428 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 23.04 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5456 _exptl_absorpt_coefficient_mu 0.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 159047 _diffrn_reflns_av_R_equivalents 0.1216 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.08 _reflns_number_total 27282 _reflns_number_gt 21828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+9.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.221(16) _refine_ls_number_reflns 27282 _refine_ls_number_parameters 1630 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.97717(3) 0.75833(3) 0.08699(2) 0.02352(16) Uani 1 1 d . . . C1 C 1.0653(2) 0.8146(2) 0.11016(15) 0.0301(11) Uani 1 1 d U . . C2 C 1.0604(2) 0.8187(2) 0.06499(15) 0.0310(11) Uani 1 1 d U . . H2 H 1.0991 0.8083 0.0484 0.037 Uiso 1 1 calc R . . C3 C 0.9981(2) 0.8383(2) 0.04502(14) 0.0289(10) Uani 1 1 d U . . C4 C 0.9389(2) 0.8521(2) 0.07048(15) 0.0309(11) Uani 1 1 d U . . H4 H 0.8974 0.8647 0.0573 0.037 Uiso 1 1 calc R . . C5 C 0.9412(3) 0.8471(2) 0.11544(15) 0.0328(11) Uani 1 1 d U . . C6 C 1.0050(3) 0.8274(2) 0.13431(15) 0.0300(10) Uani 1 1 d U . . H6 H 1.0070 0.8228 0.1638 0.036 Uiso 1 1 calc R . . C7 C 1.1339(3) 0.7944(3) 0.13079(18) 0.0427(13) Uani 1 1 d U . . H7A H 1.1661 0.8298 0.1304 0.064 Uiso 1 1 calc R . . H7B H 1.1537 0.7591 0.1152 0.064 Uiso 1 1 calc R . . H7C H 1.1254 0.7816 0.1598 0.064 Uiso 1 1 calc R . . C8 C 0.9933(3) 0.8458(3) -0.00328(14) 0.0366(12) Uani 1 1 d U . . H8A H 1.0093 0.8878 -0.0113 0.055 Uiso 1 1 calc R . . H8B H 0.9454 0.8404 -0.0122 0.055 Uiso 1 1 calc R . . H8C H 1.0221 0.8140 -0.0168 0.055 Uiso 1 1 calc R . . C9 C 0.8781(3) 0.8621(3) 0.14244(16) 0.0430(13) Uani 1 1 d U . . H9A H 0.8730 0.8298 0.1641 0.065 Uiso 1 1 calc R . . H9B H 0.8370 0.8629 0.1248 0.065 Uiso 1 1 calc R . . H9C H 0.8842 0.9033 0.1557 0.065 Uiso 1 1 calc R . . C11 C 0.9980(3) 0.6691(2) 0.11989(16) 0.0321(11) Uani 1 1 d U . . C12 C 1.0233(3) 0.6660(2) 0.07775(18) 0.0458(13) Uani 1 1 d U . . H12 H 1.0699 0.6552 0.0728 0.055 Uiso 1 1 calc R . . C13 C 0.9785(4) 0.6792(3) 0.04280(17) 0.0581(18) Uani 1 1 d U . . C14 C 0.9090(4) 0.6974(3) 0.05126(19) 0.0590(16) Uani 1 1 d U . . H14 H 0.8794 0.7070 0.0286 0.071 Uiso 1 1 calc R . . C15 C 0.8835(3) 0.7015(2) 0.0927(2) 0.0424(13) Uani 1 1 d U . . C16 C 0.9283(3) 0.6884(2) 0.12649(16) 0.0327(11) Uani 1 1 d U . . H16 H 0.9118 0.6924 0.1543 0.039 Uiso 1 1 calc R . . C17 C 1.0459(4) 0.6552(3) 0.1571(2) 0.067(2) Uani 1 1 d U . . H17A H 1.0338 0.6825 0.1807 0.101 Uiso 1 1 calc R . . H17B H 1.0937 0.6631 0.1489 0.101 Uiso 1 1 calc R . . H17C H 1.0408 0.6111 0.1655 0.101 Uiso 1 1 calc R . . C18 C 1.0051(6) 0.6759(3) -0.0027(2) 0.126(4) Uani 1 1 d U . . H18A H 1.0554 0.6766 -0.0026 0.190 Uiso 1 1 calc R . . H18B H 0.9876 0.7119 -0.0185 0.190 Uiso 1 1 calc R . . H18C H 0.9890 0.6369 -0.0157 0.190 Uiso 1 1 calc R . . C19 C 0.8077(3) 0.7211(3) 0.1019(3) 0.096(3) Uani 1 1 d U . . H19A H 0.7929 0.7523 0.0812 0.143 Uiso 1 1 calc R . . H19B H 0.8047 0.7392 0.1300 0.143 Uiso 1 1 calc R . . H19C H 0.7780 0.6841 0.1001 0.143 Uiso 1 1 calc R . . Cr2 Cr 1.04410(3) 0.57289(3) -0.20616(2) 0.01655(14) Uani 1 1 d . . . C21 C 1.1448(2) 0.62234(19) -0.20932(13) 0.0199(9) Uani 1 1 d . . . C22 C 1.1532(2) 0.56072(19) -0.19086(13) 0.0191(9) Uani 1 1 d . . . H22 H 1.1747 0.5570 -0.1643 0.023 Uiso 1 1 calc R . . C23 C 1.1296(2) 0.5046(2) -0.21205(13) 0.0226(9) Uani 1 1 d . . . C24 C 1.0952(2) 0.5116(2) -0.25158(14) 0.0259(10) Uani 1 1 d . . . H24 H 1.0781 0.4753 -0.2654 0.031 Uiso 1 1 calc R . . C25 C 1.0859(2) 0.5716(2) -0.27055(13) 0.0252(10) Uani 1 1 d . . . C26 C 1.1103(2) 0.6271(2) -0.24926(13) 0.0222(9) Uani 1 1 d . . . H26 H 1.1036 0.6672 -0.2616 0.027 Uiso 1 1 calc R . . C27 C 1.1739(2) 0.6811(2) -0.18776(14) 0.0238(10) Uani 1 1 d . . . H27A H 1.1718 0.6757 -0.1573 0.036 Uiso 1 1 calc R . . H27B H 1.1467 0.7179 -0.1958 0.036 Uiso 1 1 calc R . . H27C H 1.2218 0.6873 -0.1964 0.036 Uiso 1 1 calc R . . C28 C 1.1414(2) 0.4394(2) -0.19254(16) 0.0315(11) Uani 1 1 d . . . H28A H 1.1010 0.4129 -0.1975 0.047 Uiso 1 1 calc R . . H28B H 1.1488 0.4439 -0.1624 0.047 Uiso 1 1 calc R . . H28C H 1.1819 0.4199 -0.2053 0.047 Uiso 1 1 calc R . . C29 C 1.0502(2) 0.5793(3) -0.31383(14) 0.0363(12) Uani 1 1 d . . . H29A H 1.0848 0.5771 -0.3361 0.054 Uiso 1 1 calc R . . H29B H 1.0269 0.6201 -0.3150 0.054 Uiso 1 1 calc R . . H29C H 1.0165 0.5456 -0.3177 0.054 Uiso 1 1 calc R . . C31 C 0.9880(2) 0.6410(2) -0.16673(13) 0.0229(9) Uani 1 1 d . . . C32 C 1.0028(2) 0.5849(2) -0.14316(13) 0.0210(9) Uani 1 1 d . . . H32 H 1.0256 0.5888 -0.1171 0.025 Uiso 1 1 calc R . . C33 C 0.9840(2) 0.5229(2) -0.15779(13) 0.0205(9) Uani 1 1 d . . . C34 C 0.9494(2) 0.5178(2) -0.19717(13) 0.0229(9) Uani 1 1 d . . . H34 H 0.9366 0.4775 -0.2071 0.028 Uiso 1 1 calc R . . C35 C 0.9334(2) 0.5725(2) -0.22218(13) 0.0220(9) Uani 1 1 d . . . C36 C 0.9528(2) 0.6333(2) -0.20681(14) 0.0257(9) Uani 1 1 d . . . H36 H 0.9425 0.6694 -0.2230 0.031 Uiso 1 1 calc R . . C37 C 1.0073(3) 0.7059(2) -0.15052(16) 0.0310(11) Uani 1 1 d . . . H37A H 1.0223 0.7323 -0.1739 0.047 Uiso 1 1 calc R . . H37B H 1.0448 0.7021 -0.1302 0.047 Uiso 1 1 calc R . . H37C H 0.9673 0.7252 -0.1370 0.047 Uiso 1 1 calc R . . C38 C 0.9995(2) 0.4638(2) -0.13140(14) 0.0264(10) Uani 1 1 d . . . H38A H 0.9623 0.4571 -0.1113 0.040 Uiso 1 1 calc R . . H38B H 1.0429 0.4697 -0.1163 0.040 Uiso 1 1 calc R . . H38C H 1.0033 0.4272 -0.1499 0.040 Uiso 1 1 calc R . . C39 C 0.8951(2) 0.5647(3) -0.26414(14) 0.0339(12) Uani 1 1 d . . . H39A H 0.9086 0.5249 -0.2772 0.051 Uiso 1 1 calc R . . H39B H 0.9070 0.5996 -0.2828 0.051 Uiso 1 1 calc R . . H39C H 0.8454 0.5647 -0.2591 0.051 Uiso 1 1 calc R . . Cr3 Cr 0.95877(4) 0.42999(3) 0.07719(2) 0.02427(15) Uani 1 1 d . . . C41 C 0.9083(2) 0.5202(2) 0.0896(2) 0.0400(13) Uani 1 1 d . . . C42 C 0.9643(2) 0.5102(2) 0.11951(15) 0.0328(11) Uani 1 1 d . . . H42 H 0.9552 0.5115 0.1487 0.039 Uiso 1 1 calc R . . C43 C 1.0321(2) 0.4983(2) 0.10517(14) 0.0285(10) Uani 1 1 d . . . C44 C 1.0447(3) 0.4923(2) 0.06068(15) 0.0365(12) Uani 1 1 d . . . H44 H 1.0897 0.4823 0.0512 0.044 Uiso 1 1 calc R . . C45 C 0.9914(3) 0.5008(3) 0.03093(17) 0.0404(13) Uani 1 1 d . . . C46 C 0.9246(3) 0.5149(2) 0.04523(18) 0.0417(14) Uani 1 1 d . . . H46 H 0.8890 0.5210 0.0253 0.050 Uiso 1 1 calc R . . C47 C 0.8366(3) 0.5373(3) 0.1051(2) 0.0598(19) Uani 1 1 d . . . H47A H 0.8323 0.5831 0.1068 0.090 Uiso 1 1 calc R . . H47B H 0.8292 0.5190 0.1329 0.090 Uiso 1 1 calc R . . H47C H 0.8021 0.5208 0.0856 0.090 Uiso 1 1 calc R . . C48 C 1.0924(3) 0.4894(3) 0.13547(17) 0.0419(13) Uani 1 1 d . . . H48A H 1.1208 0.5274 0.1357 0.063 Uiso 1 1 calc R . . H48B H 1.1202 0.4535 0.1265 0.063 Uiso 1 1 calc R . . H48C H 1.0746 0.4816 0.1637 0.063 Uiso 1 1 calc R . . C49 C 1.0079(3) 0.4949(3) -0.01697(17) 0.0554(17) Uani 1 1 d . . . H49A H 0.9650 0.4899 -0.0327 0.083 Uiso 1 1 calc R . . H49B H 1.0374 0.4582 -0.0216 0.083 Uiso 1 1 calc R . . H49C H 1.0318 0.5328 -0.0265 0.083 Uiso 1 1 calc R . . C51 C 0.8741(3) 0.3670(2) 0.09605(16) 0.0350(12) Uani 1 1 d . . . C52 C 0.9322(2) 0.3577(2) 0.12326(16) 0.0313(11) Uani 1 1 d . . . H52 H 0.9263 0.3614 0.1526 0.038 Uiso 1 1 calc R . . C53 C 0.9994(2) 0.3428(2) 0.10651(15) 0.0303(11) Uani 1 1 d . . . C54 C 1.0075(3) 0.3394(2) 0.06190(16) 0.0357(12) Uani 1 1 d . . . H54 H 1.0515 0.3304 0.0507 0.043 Uiso 1 1 calc R . . C55 C 0.9509(3) 0.3493(3) 0.03372(16) 0.0393(12) Uani 1 1 d . . . C56 C 0.8840(3) 0.3636(2) 0.05150(17) 0.0390(13) Uani 1 1 d . . . H56 H 0.8461 0.3708 0.0334 0.047 Uiso 1 1 calc R . . C57 C 0.8014(3) 0.3812(3) 0.11415(19) 0.0468(15) Uani 1 1 d . . . H57A H 0.7739 0.3426 0.1143 0.070 Uiso 1 1 calc R . . H57B H 0.7786 0.4129 0.0968 0.070 Uiso 1 1 calc R . . H57C H 0.8059 0.3971 0.1428 0.070 Uiso 1 1 calc R . . C58 C 1.0599(2) 0.3308(3) 0.13609(16) 0.0364(12) Uani 1 1 d . . . H58A H 1.0551 0.3573 0.1610 0.055 Uiso 1 1 calc R . . H58B H 1.1030 0.3409 0.1218 0.055 Uiso 1 1 calc R . . H58C H 1.0602 0.2865 0.1444 0.055 Uiso 1 1 calc R . . C59 C 0.9580(4) 0.3428(3) -0.01340(16) 0.0573(17) Uani 1 1 d . . . H59A H 0.9486 0.2993 -0.0216 0.086 Uiso 1 1 calc R . . H59B H 1.0048 0.3542 -0.0218 0.086 Uiso 1 1 calc R . . H59C H 0.9251 0.3708 -0.0272 0.086 Uiso 1 1 calc R . . Cr4 Cr 0.96113(4) 0.09100(3) 0.07423(2) 0.02672(17) Uani 1 1 d . . . C61 C 1.0123(2) 0.0005(2) 0.08696(16) 0.0331(11) Uani 1 1 d . . . C62 C 0.9952(2) 0.0043(2) 0.04362(15) 0.0297(11) Uani 1 1 d . . . H62 H 1.0302 -0.0022 0.0234 0.036 Uiso 1 1 calc R . . C63 C 0.9263(2) 0.0176(2) 0.02979(16) 0.0304(11) Uani 1 1 d . . . C64 C 0.8744(2) 0.0295(2) 0.06085(16) 0.0334(12) Uani 1 1 d . . . H64 H 0.8294 0.0406 0.0520 0.040 Uiso 1 1 calc R . . C65 C 0.8886(3) 0.0251(2) 0.10479(16) 0.0360(12) Uani 1 1 d . . . C66 C 0.9587(3) 0.0113(2) 0.11750(15) 0.0359(11) Uani 1 1 d . . . H66 H 0.9696 0.0092 0.1464 0.043 Uiso 1 1 calc R . . C67 C 1.0856(3) -0.0151(3) 0.10131(17) 0.0411(13) Uani 1 1 d . . . H67A H 1.0956 -0.0593 0.0953 0.062 Uiso 1 1 calc R . . H67B H 1.0896 -0.0076 0.1315 0.062 Uiso 1 1 calc R . . H67C H 1.1184 0.0117 0.0863 0.062 Uiso 1 1 calc R . . C68 C 0.9079(3) 0.0205(3) -0.01758(16) 0.0418(13) Uani 1 1 d . . . H68A H 0.9497 0.0287 -0.0339 0.063 Uiso 1 1 calc R . . H68B H 0.8747 0.0543 -0.0224 0.063 Uiso 1 1 calc R . . H68C H 0.8879 -0.0196 -0.0263 0.063 Uiso 1 1 calc R . . C69 C 0.8322(3) 0.0364(3) 0.13796(18) 0.0479(15) Uani 1 1 d . . . H69A H 0.7960 0.0630 0.1260 0.072 Uiso 1 1 calc R . . H69B H 0.8523 0.0574 0.1623 0.072 Uiso 1 1 calc R . . H69C H 0.8125 -0.0039 0.1465 0.072 Uiso 1 1 calc R . . C71 C 1.0405(3) 0.1540(3) 0.1015(2) 0.0503(16) Uani 1 1 d . . . C72 C 1.0461(3) 0.1513(3) 0.0568(2) 0.0483(14) Uani 1 1 d . . . H72 H 1.0891 0.1406 0.0447 0.058 Uiso 1 1 calc R . . C73 C 0.9895(3) 0.1641(3) 0.02977(17) 0.0403(13) Uani 1 1 d . . . C74 C 0.9227(3) 0.1794(2) 0.04829(18) 0.0382(12) Uani 1 1 d . . . H74 H 0.8842 0.1878 0.0309 0.046 Uiso 1 1 calc R . . C75 C 0.9161(2) 0.1816(2) 0.09376(18) 0.0376(13) Uani 1 1 d . . . C76 C 0.9742(3) 0.1677(3) 0.11866(19) 0.0443(14) Uani 1 1 d . . . H76 H 0.9690 0.1674 0.1482 0.053 Uiso 1 1 calc R . . C77 C 1.1026(3) 0.1391(4) 0.1307(3) 0.081(3) Uani 1 1 d . . . H77A H 1.1159 0.1772 0.1459 0.122 Uiso 1 1 calc R . . H77B H 1.1414 0.1243 0.1138 0.122 Uiso 1 1 calc R . . H77C H 1.0894 0.1064 0.1507 0.122 Uiso 1 1 calc R . . C78 C 0.9962(4) 0.1606(3) -0.01881(19) 0.0618(18) Uani 1 1 d . . . H78A H 0.9503 0.1578 -0.0313 0.093 Uiso 1 1 calc R . . H78B H 1.0230 0.1234 -0.0265 0.093 Uiso 1 1 calc R . . H78C H 1.0194 0.1984 -0.0291 0.093 Uiso 1 1 calc R . . C79 C 0.8473(3) 0.1991(3) 0.1143(2) 0.0487(15) Uani 1 1 d . . . H79A H 0.8368 0.1690 0.1366 0.073 Uiso 1 1 calc R . . H79B H 0.8107 0.1980 0.0932 0.073 Uiso 1 1 calc R . . H79C H 0.8505 0.2415 0.1261 0.073 Uiso 1 1 calc R . . O10 O 1.1913(2) 0.51589(18) -0.08427(11) 0.0484(10) Uani 1 1 d . . . O11 O 1.16865(18) 0.59001(16) -0.03311(10) 0.0335(8) Uani 1 1 d . . . O12 O 1.18831(18) 0.60161(15) 0.07118(11) 0.0367(8) Uani 1 1 d . . . O13 O 1.27940(17) 0.60930(15) 0.02662(11) 0.0333(8) Uani 1 1 d . . . O14 O 1.2864(2) 0.49962(18) 0.11879(12) 0.0468(10) Uani 1 1 d . . . O15 O 1.2474(2) 0.39861(16) 0.11852(11) 0.0444(10) Uani 1 1 d . . . O16 O 1.3043(3) 0.3147(2) 0.04787(19) 0.091(2) Uani 1 1 d . . . O17 O 1.1893(3) 0.3014(2) 0.05369(16) 0.0853(19) Uani 1 1 d . . . O18 O 1.2174(2) 0.32000(18) -0.04476(13) 0.0543(11) Uani 1 1 d . . . O19 O 1.1354(2) 0.38656(17) -0.06821(12) 0.0529(11) Uani 1 1 d . . . C110 C 1.2013(2) 0.4884(2) -0.01039(14) 0.0252(10) Uani 1 1 d . . . C111 C 1.2231(2) 0.5099(2) 0.03085(14) 0.0232(10) Uani 1 1 d . . . C112 C 1.2371(2) 0.4557(2) 0.05530(14) 0.0248(10) Uani 1 1 d . . . C113 C 1.2268(3) 0.4006(2) 0.03001(15) 0.0341(12) Uani 1 1 d . . . C114 C 1.2049(2) 0.4195(2) -0.01029(15) 0.0284(10) Uani 1 1 d . . . C115 C 1.1874(3) 0.5302(2) -0.04586(16) 0.0332(12) Uani 1 1 d . . . C116 C 1.2268(2) 0.5777(2) 0.04546(15) 0.0272(10) Uani 1 1 d . . . C117 C 1.2609(2) 0.4554(2) 0.10008(15) 0.0258(10) Uani 1 1 d . . . C118 C 1.2445(6) 0.3346(3) 0.04434(19) 0.070(2) Uani 1 1 d . . . C119 C 1.1874(3) 0.3710(2) -0.04303(16) 0.0335(12) Uani 1 1 d . . . C120 C 1.1694(3) 0.6392(2) -0.06560(16) 0.0385(13) Uani 1 1 d . . . H12A H 1.2136 0.6384 -0.0803 0.058 Uiso 1 1 calc R . . H12B H 1.1629 0.6804 -0.0525 0.058 Uiso 1 1 calc R . . H12C H 1.1322 0.6315 -0.0856 0.058 Uiso 1 1 calc R . . C121 C 1.2813(3) 0.6780(2) 0.03485(18) 0.0395(13) Uani 1 1 d . . . H12D H 1.2397 0.6976 0.0235 0.059 Uiso 1 1 calc R . . H12E H 1.3219 0.6963 0.0214 0.059 Uiso 1 1 calc R . . H12F H 1.2835 0.6854 0.0651 0.059 Uiso 1 1 calc R . . C122 C 1.2669(3) 0.3891(3) 0.16258(15) 0.0405(13) Uani 1 1 d . . . H12G H 1.2882 0.4275 0.1734 0.061 Uiso 1 1 calc R . . H12H H 1.2997 0.3542 0.1645 0.061 Uiso 1 1 calc R . . H12I H 1.2258 0.3792 0.1791 0.061 Uiso 1 1 calc R . . C123 C 1.2280(7) 0.2445(4) 0.0812(3) 0.147(5) Uani 1 1 d U . . H12J H 1.2777 0.2465 0.0765 0.220 Uiso 1 1 calc R . . H12K H 1.2106 0.2035 0.0720 0.220 Uiso 1 1 calc R . . H12L H 1.2182 0.2503 0.1110 0.220 Uiso 1 1 calc R . . C124 C 1.1186(4) 0.3361(3) -0.09961(18) 0.0566(18) Uani 1 1 d . . . H12M H 1.1571 0.3312 -0.1191 0.085 Uiso 1 1 calc R . . H12N H 1.0772 0.3480 -0.1152 0.085 Uiso 1 1 calc R . . H12O H 1.1105 0.2964 -0.0850 0.085 Uiso 1 1 calc R . . O20 O 0.66997(16) 0.69853(14) 0.01824(9) 0.0264(7) Uani 1 1 d . . . O21 O 0.65267(16) 0.63073(14) 0.07345(9) 0.0249(7) Uani 1 1 d . . . O22 O 0.80300(18) 0.68332(15) -0.03232(10) 0.0328(8) Uani 1 1 d . . . O23 O 0.78165(17) 0.62490(16) -0.09068(9) 0.0326(8) Uani 1 1 d . . . O24 O 0.85747(18) 0.4975(2) -0.07353(13) 0.0540(11) Uani 1 1 d . . . O25 O 0.75649(16) 0.46576(16) -0.10223(9) 0.0304(8) Uani 1 1 d . . . O26 O 0.75889(18) 0.38027(15) -0.02583(10) 0.0338(8) Uani 1 1 d . . . O27 O 0.67473(17) 0.38590(14) 0.02370(11) 0.0315(8) Uani 1 1 d . . . O28 O 0.57150(16) 0.50336(15) 0.05575(10) 0.0296(7) Uani 1 1 d . . . O29 O 0.66980(16) 0.48243(15) 0.09226(9) 0.0265(7) Uani 1 1 d . . . C130 C 0.6989(2) 0.5873(2) 0.01132(13) 0.0198(9) Uani 1 1 d . . . C131 C 0.7412(2) 0.5841(2) -0.02612(13) 0.0202(9) Uani 1 1 d . . . C132 C 0.7508(2) 0.5200(2) -0.03721(13) 0.0219(9) Uani 1 1 d . . . C134 C 0.6826(2) 0.5237(2) 0.02279(14) 0.0215(9) Uani 1 1 d . . . C133 C 0.7149(2) 0.4821(2) -0.00617(14) 0.0215(9) Uani 1 1 d . . . C135 C 0.6736(2) 0.6445(2) 0.03282(13) 0.0206(9) Uani 1 1 d . . . C136 C 0.7774(2) 0.6366(2) -0.04826(13) 0.0207(9) Uani 1 1 d . . . C137 C 0.7941(2) 0.4942(2) -0.07210(15) 0.0253(10) Uani 1 1 d . . . C138 C 0.7188(2) 0.4121(2) -0.00475(14) 0.0248(10) Uani 1 1 d . . . C139 C 0.6341(2) 0.5030(2) 0.05792(13) 0.0216(9) Uani 1 1 d . . . C140 C 0.6201(2) 0.6822(2) 0.09658(13) 0.0261(10) Uani 1 1 d . . . H14A H 0.6517 0.7179 0.0981 0.039 Uiso 1 1 calc R . . H14B H 0.6089 0.6680 0.1249 0.039 Uiso 1 1 calc R . . H14C H 0.5779 0.6950 0.0822 0.039 Uiso 1 1 calc R . . C141 C 0.8258(3) 0.6674(3) -0.11477(17) 0.0469(15) Uani 1 1 d . . . H14D H 0.8031 0.7083 -0.1176 0.070 Uiso 1 1 calc R . . H14E H 0.8341 0.6496 -0.1426 0.070 Uiso 1 1 calc R . . H14F H 0.8697 0.6728 -0.1002 0.070 Uiso 1 1 calc R . . C142 C 0.7964(3) 0.4357(3) -0.13663(16) 0.0465(15) Uani 1 1 d . . . H14G H 0.8247 0.4674 -0.1507 0.070 Uiso 1 1 calc R . . H14H H 0.7647 0.4169 -0.1569 0.070 Uiso 1 1 calc R . . H14I H 0.8262 0.4029 -0.1250 0.070 Uiso 1 1 calc R . . C143 C 0.6829(3) 0.3182(2) 0.03076(16) 0.0349(12) Uani 1 1 d . . . H14J H 0.6637 0.2951 0.0070 0.052 Uiso 1 1 calc R . . H14K H 0.6586 0.3062 0.0564 0.052 Uiso 1 1 calc R . . H14L H 0.7318 0.3082 0.0336 0.052 Uiso 1 1 calc R . . C144 C 0.6276(3) 0.4536(2) 0.12556(15) 0.0364(12) Uani 1 1 d . . . H14M H 0.5926 0.4836 0.1349 0.055 Uiso 1 1 calc R . . H14N H 0.6570 0.4422 0.1492 0.055 Uiso 1 1 calc R . . H14O H 0.6050 0.4158 0.1146 0.055 Uiso 1 1 calc R . . O30 O 1.0746(2) 0.20749(18) -0.17863(12) 0.0473(10) Uani 1 1 d . . . O31 O 1.16176(16) 0.26495(16) -0.20618(11) 0.0366(8) Uani 1 1 d . . . O32 O 0.8785(2) 0.25645(18) -0.18740(11) 0.0434(9) Uani 1 1 d . . . O33 O 0.9663(3) 0.2912(2) -0.14756(11) 0.0712(14) Uani 1 1 d . . . O34 O 0.84736(18) 0.38997(17) -0.23024(10) 0.0360(8) Uani 1 1 d . . . O35 O 0.85416(17) 0.35837(17) -0.29803(10) 0.0375(8) Uani 1 1 d . . . O36 O 0.97044(18) 0.43621(15) -0.32731(10) 0.0362(8) Uani 1 1 d . . . O37 O 1.04636(17) 0.36571(14) -0.35463(9) 0.0293(7) Uani 1 1 d . . . O38 O 1.15954(17) 0.25773(16) -0.30154(11) 0.0398(8) Uani 1 1 d . . . O39 O 1.16640(17) 0.36422(15) -0.30102(10) 0.0320(8) Uani 1 1 d . . . C150 C 1.0494(2) 0.2890(2) -0.22922(13) 0.0228(9) Uani 1 1 d . . . C151 C 0.9778(2) 0.3044(2) -0.22105(13) 0.0203(9) Uani 1 1 d . . . C152 C 0.9526(2) 0.34086(19) -0.25534(12) 0.0201(9) Uani 1 1 d . . . C153 C 1.0086(2) 0.3494(2) -0.28460(13) 0.0234(9) Uani 1 1 d . . . C154 C 1.0677(2) 0.31712(19) -0.26893(13) 0.0208(9) Uani 1 1 d . . . C155 C 1.0939(2) 0.2498(2) -0.20170(14) 0.0277(10) Uani 1 1 d . . . C156 C 0.9346(3) 0.2818(2) -0.18499(14) 0.0320(12) Uani 1 1 d . . . C157 C 0.8804(2) 0.3660(2) -0.25875(14) 0.0237(10) Uani 1 1 d . . . C158 C 1.0048(2) 0.3887(2) -0.32332(14) 0.0246(10) Uani 1 1 d . . . C159 C 1.1352(2) 0.3091(2) -0.29173(14) 0.0245(10) Uani 1 1 d . . . C160 C 1.2109(3) 0.2232(3) -0.18457(19) 0.0461(15) Uani 1 1 d . . . H16A H 1.2013 0.2234 -0.1545 0.069 Uiso 1 1 calc R . . H16B H 1.2578 0.2381 -0.1895 0.069 Uiso 1 1 calc R . . H16C H 1.2061 0.1804 -0.1954 0.069 Uiso 1 1 calc R . . C161 C 0.9316(6) 0.2592(5) -0.1118(2) 0.122(4) Uani 1 1 d . . . H16D H 0.8862 0.2779 -0.1073 0.183 Uiso 1 1 calc R . . H16E H 0.9594 0.2643 -0.0864 0.183 Uiso 1 1 calc R . . H16F H 0.9265 0.2144 -0.1181 0.183 Uiso 1 1 calc R . . C162 C 0.7880(3) 0.3890(3) -0.30643(17) 0.0482(15) Uani 1 1 d . . . H16G H 0.7511 0.3655 -0.2927 0.072 Uiso 1 1 calc R . . H16H H 0.7797 0.3900 -0.3367 0.072 Uiso 1 1 calc R . . H16I H 0.7890 0.4321 -0.2956 0.072 Uiso 1 1 calc R . . C163 C 1.0563(3) 0.4083(2) -0.39114(14) 0.0359(12) Uani 1 1 d . . . H16J H 1.0114 0.4193 -0.4030 0.054 Uiso 1 1 calc R . . H16K H 1.0840 0.3869 -0.4124 0.054 Uiso 1 1 calc R . . H16L H 1.0799 0.4465 -0.3820 0.054 Uiso 1 1 calc R . . C164 C 1.2222(3) 0.3600(3) -0.33296(17) 0.0429(13) Uani 1 1 d . . . H16M H 1.2612 0.3366 -0.3213 0.064 Uiso 1 1 calc R . . H16N H 1.2371 0.4024 -0.3407 0.064 Uiso 1 1 calc R . . H16O H 1.2049 0.3382 -0.3578 0.064 Uiso 1 1 calc R . . O40 O 1.0213(2) 0.52092(17) 0.28127(11) 0.0441(9) Uani 1 1 d . . . O41 O 0.93749(17) 0.50580(15) 0.23314(11) 0.0341(8) Uani 1 1 d . . . O42 O 1.19491(16) 0.39013(16) 0.26541(11) 0.0325(8) Uani 1 1 d . . . O43 O 1.14263(17) 0.47534(16) 0.23678(11) 0.0364(8) Uani 1 1 d . . . O44 O 1.1253(2) 0.23236(17) 0.27684(10) 0.0420(9) Uani 1 1 d . . . O45 O 1.15708(16) 0.27062(15) 0.21314(9) 0.0288(7) Uani 1 1 d . . . O46 O 0.9879(2) 0.19942(18) 0.22476(12) 0.0496(10) Uani 1 1 d . . . O47 O 0.88984(19) 0.24342(18) 0.25122(11) 0.0437(9) Uani 1 1 d . . . O48 O 0.83633(18) 0.3720(2) 0.22134(12) 0.0495(10) Uani 1 1 d . . . O49 O 0.86011(17) 0.40782(19) 0.28689(11) 0.0431(9) Uani 1 1 d . . . C170 C 1.0059(2) 0.4163(2) 0.25067(14) 0.0246(10) Uani 1 1 d . . . C171 C 1.0733(2) 0.3861(2) 0.25081(14) 0.0260(10) Uani 1 1 d . . . C172 C 1.0614(2) 0.3199(2) 0.24721(13) 0.0216(9) Uani 1 1 d . . . C173 C 0.9884(2) 0.3095(2) 0.24490(13) 0.0264(10) Uani 1 1 d . . . C174 C 0.9545(2) 0.3689(2) 0.24761(13) 0.0249(9) Uani 1 1 d . . . C175 C 0.9906(2) 0.4861(2) 0.25737(14) 0.0274(10) Uani 1 1 d . . . C176 C 1.1431(2) 0.4153(2) 0.25251(13) 0.0240(10) Uani 1 1 d . . . C177 C 1.1165(2) 0.2694(2) 0.24819(14) 0.0272(10) Uani 1 1 d . . . C178 C 0.9572(3) 0.2458(2) 0.23895(14) 0.0342(11) Uani 1 1 d . . . C179 C 0.8778(2) 0.3822(2) 0.24893(15) 0.0283(10) Uani 1 1 d . . . C180 C 0.9119(3) 0.5699(3) 0.24141(19) 0.0513(15) Uani 1 1 d . . . H18D H 0.8847 0.5699 0.2672 0.077 Uiso 1 1 calc R . . H18E H 0.8832 0.5837 0.2180 0.077 Uiso 1 1 calc R . . H18F H 0.9510 0.5985 0.2446 0.077 Uiso 1 1 calc R . . C181 C 1.2065(2) 0.5111(2) 0.24134(18) 0.0399(13) Uani 1 1 d . . . H18G H 1.2180 0.5150 0.2711 0.060 Uiso 1 1 calc R . . H18H H 1.2005 0.5531 0.2293 0.060 Uiso 1 1 calc R . . H18I H 1.2438 0.4892 0.2267 0.060 Uiso 1 1 calc R . . C182 C 1.2155(2) 0.2265(2) 0.21390(16) 0.0326(11) Uani 1 1 d . . . H18J H 1.2444 0.2353 0.2383 0.049 Uiso 1 1 calc R . . H18K H 1.2428 0.2316 0.1884 0.049 Uiso 1 1 calc R . . H18L H 1.1982 0.1833 0.2155 0.049 Uiso 1 1 calc R . . C183 C 0.8562(4) 0.1820(3) 0.24378(19) 0.0622(19) Uani 1 1 d . . . H18M H 0.8529 0.1743 0.2136 0.093 Uiso 1 1 calc R . . H18N H 0.8100 0.1824 0.2560 0.093 Uiso 1 1 calc R . . H18O H 0.8835 0.1486 0.2568 0.093 Uiso 1 1 calc R . . C184 C 0.7864(3) 0.4237(4) 0.2914(2) 0.073(2) Uani 1 1 d . . . H18P H 0.7743 0.4568 0.2714 0.109 Uiso 1 1 calc R . . H18Q H 0.7776 0.4385 0.3199 0.109 Uiso 1 1 calc R . . H18R H 0.7585 0.3863 0.2859 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0250(3) 0.0275(4) 0.0181(3) -0.0024(3) 0.0012(3) 0.0031(3) C1 0.036(2) 0.030(3) 0.025(2) -0.001(2) -0.005(2) -0.006(2) C2 0.030(2) 0.039(3) 0.024(2) -0.005(2) 0.0016(19) 0.001(2) C3 0.036(3) 0.028(3) 0.023(2) -0.004(2) -0.0017(19) 0.000(2) C4 0.031(2) 0.036(3) 0.026(2) -0.001(2) -0.0009(19) -0.003(2) C5 0.044(3) 0.031(3) 0.023(2) 0.001(2) 0.007(2) 0.000(2) C6 0.041(3) 0.028(3) 0.020(2) 0.000(2) 0.001(2) 0.001(2) C7 0.034(3) 0.045(3) 0.048(3) 0.000(3) -0.013(2) -0.003(2) C8 0.039(3) 0.047(3) 0.024(2) 0.000(2) 0.005(2) 0.003(2) C9 0.055(3) 0.049(3) 0.026(3) -0.002(2) 0.005(2) 0.019(3) C11 0.035(3) 0.024(2) 0.037(3) 0.001(2) -0.012(2) -0.001(2) C12 0.041(3) 0.037(3) 0.059(3) -0.003(3) 0.025(3) 0.009(2) C13 0.123(6) 0.027(3) 0.025(3) -0.001(2) 0.012(3) 0.002(3) C14 0.099(5) 0.040(3) 0.039(3) -0.006(3) -0.032(3) -0.007(3) C15 0.034(3) 0.029(3) 0.064(4) -0.003(3) -0.014(2) -0.005(2) C16 0.041(3) 0.030(3) 0.026(2) -0.006(2) 0.009(2) -0.005(2) C17 0.075(4) 0.039(3) 0.088(5) 0.026(3) -0.048(4) -0.010(3) C18 0.287(12) 0.041(4) 0.051(4) -0.005(3) 0.069(6) 0.007(6) C19 0.032(3) 0.059(5) 0.195(9) 0.020(5) -0.004(4) 0.005(3) Cr2 0.0180(3) 0.0163(3) 0.0153(3) -0.0007(3) 0.0030(3) 0.0001(3) C21 0.024(2) 0.017(2) 0.018(2) -0.0052(18) 0.0063(18) -0.0003(17) C22 0.018(2) 0.019(2) 0.020(2) 0.0011(17) 0.0019(17) -0.0018(17) C23 0.026(2) 0.021(2) 0.020(2) -0.0064(18) 0.0111(18) -0.0008(18) C24 0.024(2) 0.028(2) 0.026(2) -0.010(2) 0.0122(19) -0.0071(19) C25 0.021(2) 0.037(3) 0.018(2) 0.005(2) 0.0047(17) -0.007(2) C26 0.025(2) 0.023(2) 0.019(2) 0.0030(18) 0.0069(18) 0.0020(18) C27 0.026(2) 0.019(2) 0.026(2) -0.0038(19) 0.0023(19) -0.0071(18) C28 0.026(2) 0.020(2) 0.048(3) 0.002(2) 0.008(2) 0.0017(19) C29 0.030(3) 0.059(3) 0.020(2) 0.000(2) 0.002(2) -0.010(3) C31 0.024(2) 0.023(2) 0.023(2) -0.0058(18) 0.0061(18) 0.0021(19) C32 0.021(2) 0.025(2) 0.017(2) -0.0028(18) 0.0044(17) 0.0016(18) C33 0.020(2) 0.020(2) 0.021(2) 0.0026(18) 0.0084(17) 0.0031(18) C34 0.021(2) 0.023(2) 0.024(2) -0.0053(18) 0.0066(18) -0.0040(18) C35 0.0151(19) 0.029(2) 0.022(2) -0.0031(19) 0.0052(16) 0.0021(18) C36 0.023(2) 0.027(2) 0.027(2) 0.003(2) 0.005(2) 0.0060(19) C37 0.033(3) 0.024(2) 0.036(3) -0.007(2) 0.006(2) 0.003(2) C38 0.026(2) 0.027(2) 0.027(2) 0.011(2) 0.0092(19) 0.0024(19) C39 0.023(2) 0.054(3) 0.024(2) -0.005(2) -0.0043(19) -0.003(2) Cr3 0.0233(3) 0.0301(4) 0.0195(3) 0.0021(3) -0.0020(3) -0.0040(3) C41 0.026(2) 0.026(3) 0.068(4) -0.006(3) 0.004(3) -0.008(2) C42 0.025(2) 0.046(3) 0.027(2) -0.004(2) 0.003(2) -0.003(2) C43 0.026(2) 0.038(3) 0.022(2) 0.001(2) 0.0004(19) -0.011(2) C44 0.032(3) 0.049(3) 0.029(3) -0.001(2) -0.001(2) -0.014(3) C45 0.049(3) 0.039(3) 0.033(3) 0.005(2) -0.004(2) -0.014(3) C46 0.052(3) 0.028(3) 0.045(3) 0.010(2) -0.028(3) -0.003(3) C47 0.033(3) 0.031(3) 0.115(6) -0.022(3) -0.001(3) -0.008(2) C48 0.037(3) 0.052(4) 0.037(3) -0.010(3) -0.011(2) -0.010(3) C49 0.062(4) 0.071(4) 0.033(3) 0.014(3) 0.001(3) -0.022(3) C51 0.030(3) 0.037(3) 0.037(3) 0.011(2) -0.005(2) -0.005(2) C52 0.031(3) 0.034(3) 0.029(3) 0.008(2) -0.001(2) -0.006(2) C53 0.030(3) 0.037(3) 0.024(2) 0.001(2) -0.004(2) 0.000(2) C54 0.033(3) 0.042(3) 0.033(3) -0.002(2) 0.001(2) -0.002(2) C55 0.049(3) 0.038(3) 0.031(3) -0.003(2) -0.006(3) -0.006(3) C56 0.038(3) 0.036(3) 0.044(3) 0.006(2) -0.018(2) 0.000(2) C57 0.031(3) 0.046(3) 0.062(4) 0.023(3) 0.002(3) -0.004(2) C58 0.033(3) 0.041(3) 0.036(3) 0.001(2) -0.004(2) 0.008(2) C59 0.084(5) 0.059(4) 0.029(3) -0.011(3) -0.011(3) 0.012(4) Cr4 0.0216(3) 0.0294(4) 0.0291(4) -0.0088(3) -0.0026(3) -0.0018(3) C61 0.029(2) 0.037(3) 0.033(3) -0.002(2) 0.001(2) 0.001(2) C62 0.026(2) 0.030(3) 0.033(3) -0.006(2) -0.001(2) 0.004(2) C63 0.023(2) 0.033(3) 0.035(3) -0.008(2) -0.002(2) -0.001(2) C64 0.020(2) 0.033(3) 0.047(3) -0.010(2) -0.002(2) 0.002(2) C65 0.035(3) 0.036(3) 0.037(3) -0.007(2) 0.001(2) -0.006(2) C66 0.034(3) 0.046(3) 0.028(3) -0.003(2) -0.006(2) 0.001(3) C67 0.034(3) 0.050(3) 0.039(3) 0.003(3) -0.003(2) 0.002(3) C68 0.035(3) 0.053(3) 0.038(3) -0.012(3) -0.009(2) -0.002(3) C69 0.038(3) 0.056(4) 0.050(3) -0.005(3) 0.018(3) -0.004(3) C71 0.034(3) 0.048(3) 0.069(4) -0.033(3) -0.014(3) 0.008(3) C72 0.029(3) 0.042(3) 0.074(4) -0.008(3) 0.005(3) -0.008(3) C73 0.046(3) 0.033(3) 0.043(3) -0.003(2) 0.011(3) -0.005(2) C74 0.039(3) 0.029(3) 0.047(3) 0.001(2) -0.008(3) -0.003(2) C75 0.026(3) 0.034(3) 0.053(3) -0.015(3) 0.008(2) -0.002(2) C76 0.031(3) 0.054(4) 0.048(3) -0.021(3) -0.011(2) 0.007(3) C77 0.044(4) 0.085(5) 0.115(6) -0.068(5) -0.037(4) 0.019(4) C78 0.081(5) 0.045(4) 0.059(4) 0.017(3) 0.022(4) -0.007(3) C79 0.046(3) 0.027(3) 0.073(4) -0.004(3) 0.008(3) 0.008(3) O10 0.073(3) 0.042(2) 0.030(2) 0.0048(17) 0.0055(19) 0.005(2) O11 0.041(2) 0.0314(19) 0.0283(18) 0.0105(15) -0.0041(15) 0.0044(16) O12 0.047(2) 0.0228(18) 0.040(2) -0.0022(16) 0.0112(17) 0.0059(15) O13 0.0296(18) 0.0233(17) 0.047(2) 0.0012(15) 0.0044(16) -0.0022(14) O14 0.057(2) 0.040(2) 0.044(2) 0.0051(18) -0.0174(19) -0.0212(19) O15 0.082(3) 0.0232(19) 0.0279(19) 0.0032(15) -0.0087(19) -0.0067(18) O16 0.134(5) 0.028(2) 0.112(5) -0.006(3) -0.060(4) 0.019(3) O17 0.136(5) 0.027(2) 0.093(4) 0.011(2) 0.080(4) 0.017(3) O18 0.062(3) 0.036(2) 0.065(3) -0.017(2) -0.002(2) 0.006(2) O19 0.087(3) 0.0272(19) 0.045(2) -0.0086(17) -0.021(2) 0.013(2) C110 0.025(2) 0.029(3) 0.021(2) 0.005(2) 0.0027(19) 0.000(2) C111 0.016(2) 0.030(3) 0.024(2) -0.002(2) 0.0056(18) 0.0019(18) C112 0.018(2) 0.029(2) 0.028(2) 0.000(2) 0.0034(18) 0.0035(19) C113 0.053(3) 0.024(3) 0.025(3) -0.009(2) 0.014(2) 0.001(2) C114 0.037(3) 0.021(2) 0.027(2) -0.002(2) 0.007(2) 0.002(2) C115 0.028(3) 0.035(3) 0.036(3) 0.000(2) 0.009(2) 0.002(2) C116 0.027(2) 0.026(3) 0.029(3) 0.003(2) -0.002(2) 0.000(2) C117 0.020(2) 0.024(2) 0.034(3) -0.003(2) 0.0033(19) 0.0030(19) C118 0.159(8) 0.022(3) 0.030(3) -0.002(3) 0.010(4) 0.014(4) C119 0.034(3) 0.031(3) 0.036(3) 0.009(2) 0.012(2) 0.002(2) C120 0.048(3) 0.031(3) 0.037(3) 0.019(2) -0.003(2) -0.003(2) C121 0.049(3) 0.018(3) 0.052(3) -0.001(2) -0.001(3) -0.006(2) C122 0.052(3) 0.043(3) 0.027(3) 0.004(2) -0.008(2) -0.003(3) C123 0.321(15) 0.040(4) 0.079(6) 0.031(4) 0.025(8) 0.027(7) C124 0.106(5) 0.024(3) 0.039(3) -0.007(2) -0.020(3) 0.008(3) O20 0.0335(18) 0.0231(17) 0.0225(16) 0.0023(13) 0.0045(14) 0.0031(14) O21 0.0327(17) 0.0225(16) 0.0196(15) -0.0012(13) 0.0049(14) 0.0018(13) O22 0.042(2) 0.0267(18) 0.0301(18) 0.0023(15) 0.0042(15) -0.0099(15) O23 0.0422(19) 0.040(2) 0.0158(15) 0.0029(14) 0.0120(14) -0.0126(16) O24 0.0277(19) 0.076(3) 0.058(3) -0.035(2) 0.0092(18) 0.0008(19) O25 0.0279(17) 0.042(2) 0.0209(17) -0.0131(15) 0.0109(14) 0.0016(15) O26 0.046(2) 0.0223(17) 0.0332(19) -0.0058(15) 0.0052(16) 0.0045(16) O27 0.0377(19) 0.0176(16) 0.0391(19) 0.0023(15) 0.0080(16) 0.0020(14) O28 0.0271(17) 0.0348(19) 0.0270(17) 0.0007(15) 0.0048(14) -0.0038(15) O29 0.0312(17) 0.0275(17) 0.0206(16) 0.0077(14) 0.0056(13) 0.0040(14) C130 0.024(2) 0.022(2) 0.014(2) 0.0024(17) -0.0001(17) -0.0020(18) C131 0.018(2) 0.022(2) 0.020(2) -0.0022(18) 0.0002(17) -0.0002(17) C132 0.015(2) 0.030(3) 0.021(2) -0.0007(19) 0.0005(17) 0.0024(18) C134 0.020(2) 0.024(2) 0.021(2) 0.0011(19) -0.0013(18) 0.0049(18) C133 0.021(2) 0.022(2) 0.022(2) -0.0014(19) -0.0021(18) 0.0012(18) C135 0.020(2) 0.023(2) 0.018(2) -0.0031(18) 0.0023(17) -0.0038(18) C136 0.021(2) 0.026(2) 0.015(2) -0.0029(18) 0.0062(17) 0.0010(19) C137 0.023(2) 0.025(2) 0.028(2) -0.001(2) 0.0039(19) 0.0025(19) C138 0.026(2) 0.024(2) 0.024(2) 0.000(2) -0.0068(19) 0.0020(19) C139 0.027(2) 0.018(2) 0.020(2) -0.0013(18) 0.0065(18) 0.0001(19) C140 0.027(2) 0.035(3) 0.016(2) -0.0056(19) 0.0052(18) 0.004(2) C141 0.055(3) 0.050(4) 0.035(3) 0.010(3) 0.025(3) -0.014(3) C142 0.048(3) 0.060(4) 0.031(3) -0.021(3) 0.016(2) 0.001(3) C143 0.050(3) 0.022(3) 0.033(3) 0.002(2) -0.004(2) -0.009(2) C144 0.048(3) 0.033(3) 0.028(3) 0.011(2) 0.018(2) 0.011(2) O30 0.046(2) 0.046(2) 0.049(2) 0.026(2) -0.0169(19) -0.0055(19) O31 0.0317(18) 0.0328(19) 0.045(2) 0.0129(17) -0.0142(16) 0.0055(15) O32 0.054(2) 0.045(2) 0.0317(19) 0.0022(17) 0.0099(17) -0.009(2) O33 0.089(3) 0.104(4) 0.020(2) -0.008(2) -0.010(2) -0.016(3) O34 0.0373(19) 0.040(2) 0.0307(19) -0.0101(16) 0.0010(16) 0.0090(16) O35 0.0343(18) 0.053(2) 0.0254(18) -0.0114(17) -0.0094(15) 0.0144(17) O36 0.054(2) 0.0238(18) 0.0305(18) 0.0068(14) -0.0043(16) 0.0131(17) O37 0.0364(18) 0.0290(17) 0.0226(16) 0.0063(13) -0.0019(15) 0.0035(15) O38 0.0390(19) 0.0276(19) 0.053(2) -0.0022(17) 0.0097(17) 0.0047(16) O39 0.0334(18) 0.0254(17) 0.0372(19) 0.0003(15) 0.0000(15) -0.0049(14) C150 0.032(2) 0.018(2) 0.018(2) -0.0046(17) -0.0082(19) -0.0047(19) C151 0.027(2) 0.019(2) 0.015(2) -0.0044(17) -0.0074(17) -0.0010(18) C152 0.027(2) 0.017(2) 0.016(2) -0.0045(16) -0.0054(18) -0.0015(18) C153 0.028(2) 0.020(2) 0.022(2) -0.0040(18) -0.0064(18) 0.0035(18) C154 0.024(2) 0.015(2) 0.023(2) -0.0039(18) -0.0076(18) 0.0004(17) C155 0.039(3) 0.022(2) 0.022(2) -0.007(2) -0.008(2) 0.001(2) C156 0.050(3) 0.028(3) 0.018(2) -0.0028(19) -0.004(2) 0.011(2) C157 0.031(2) 0.017(2) 0.024(2) -0.0019(19) -0.002(2) 0.0011(19) C158 0.030(2) 0.017(2) 0.027(2) -0.0063(19) -0.007(2) 0.0031(19) C159 0.027(2) 0.025(2) 0.022(2) 0.002(2) -0.0095(19) -0.0006(19) C160 0.035(3) 0.039(3) 0.064(4) 0.002(3) -0.023(3) 0.006(2) C161 0.182(10) 0.166(10) 0.017(3) 0.013(5) 0.014(5) -0.033(8) C162 0.034(3) 0.070(4) 0.041(3) -0.004(3) -0.010(2) 0.024(3) C163 0.043(3) 0.043(3) 0.022(2) 0.010(2) -0.007(2) -0.007(2) C164 0.042(3) 0.043(3) 0.043(3) -0.001(3) 0.008(3) -0.008(3) O40 0.055(2) 0.034(2) 0.044(2) -0.0100(17) -0.0226(19) 0.0015(17) O41 0.0367(19) 0.0256(18) 0.040(2) -0.0006(15) -0.0078(15) 0.0095(15) O42 0.0235(17) 0.0332(19) 0.041(2) 0.0120(16) -0.0041(15) 0.0002(14) O43 0.0282(18) 0.0284(18) 0.053(2) 0.0140(17) -0.0073(16) -0.0054(15) O44 0.057(2) 0.038(2) 0.0310(19) 0.0185(17) 0.0118(17) 0.0172(18) O45 0.0296(17) 0.0325(18) 0.0244(17) 0.0054(14) -0.0002(14) 0.0089(14) O46 0.068(3) 0.033(2) 0.048(2) -0.0068(18) -0.001(2) -0.010(2) O47 0.046(2) 0.048(2) 0.037(2) 0.0056(18) -0.0027(17) -0.0232(18) O48 0.0272(19) 0.077(3) 0.044(2) -0.004(2) -0.0106(17) -0.0079(19) O49 0.0227(17) 0.072(3) 0.035(2) -0.0086(19) 0.0032(15) 0.0051(17) C170 0.025(2) 0.029(2) 0.019(2) 0.0043(19) -0.0006(18) 0.0005(19) C171 0.030(2) 0.031(3) 0.016(2) 0.005(2) 0.0008(19) 0.006(2) C172 0.024(2) 0.028(2) 0.013(2) 0.0018(18) -0.0013(17) -0.0043(18) C173 0.038(3) 0.027(2) 0.014(2) 0.0011(19) 0.0006(19) -0.003(2) C174 0.025(2) 0.034(3) 0.017(2) 0.0020(19) -0.0023(19) -0.005(2) C175 0.027(2) 0.031(3) 0.024(2) 0.003(2) -0.005(2) -0.001(2) C176 0.025(2) 0.029(3) 0.018(2) 0.0026(19) -0.0014(18) -0.0037(19) C177 0.030(2) 0.030(3) 0.022(2) 0.001(2) -0.0008(19) -0.005(2) C178 0.043(3) 0.034(3) 0.025(2) 0.004(2) -0.006(2) -0.016(3) C179 0.023(2) 0.038(3) 0.024(2) 0.001(2) -0.001(2) -0.002(2) C180 0.053(4) 0.045(3) 0.056(4) -0.001(3) -0.003(3) 0.017(3) C181 0.025(3) 0.037(3) 0.058(4) 0.004(3) 0.000(2) -0.007(2) C182 0.031(3) 0.031(3) 0.036(3) 0.000(2) 0.003(2) 0.010(2) C183 0.077(5) 0.062(4) 0.047(4) 0.009(3) -0.014(3) -0.038(4) C184 0.035(3) 0.123(6) 0.060(4) -0.008(5) 0.007(3) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C16 2.127(5) . ? Cr1 C14 2.133(6) . ? Cr1 C6 2.133(5) . ? Cr1 C12 2.136(5) . ? Cr1 C2 2.139(5) . ? Cr1 C4 2.150(5) . ? Cr1 C15 2.150(5) . ? Cr1 C13 2.153(5) . ? Cr1 C3 2.161(5) . ? Cr1 C11 2.164(5) . ? Cr1 C5 2.167(5) . ? Cr1 C1 2.173(5) . ? C1 C6 1.402(7) . ? C1 C2 1.420(6) . ? C1 C7 1.518(7) . ? C2 C3 1.403(6) . ? C2 H2 0.9300 . ? C3 C4 1.411(6) . ? C3 C8 1.523(6) . ? C4 C5 1.412(6) . ? C4 H4 0.9300 . ? C5 C6 1.413(7) . ? C5 C9 1.502(7) . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C16 1.403(7) . ? C11 C12 1.406(7) . ? C11 C17 1.509(7) . ? C12 C13 1.415(9) . ? C12 H12 0.9300 . ? C13 C14 1.402(10) . ? C13 C18 1.513(8) . ? C14 C15 1.389(9) . ? C14 H14 0.9300 . ? C15 C16 1.388(7) . ? C15 C19 1.527(8) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Cr2 C32 2.139(4) . ? Cr2 C24 2.146(4) . ? Cr2 C36 2.149(4) . ? Cr2 C22 2.149(4) . ? Cr2 C34 2.158(4) . ? Cr2 C31 2.164(4) . ? Cr2 C26 2.166(4) . ? Cr2 C33 2.166(4) . ? Cr2 C25 2.168(4) . ? Cr2 C35 2.169(4) . ? Cr2 C23 2.171(4) . ? Cr2 C21 2.180(4) . ? C21 C26 1.416(6) . ? C21 C22 1.418(6) . ? C21 C27 1.506(6) . ? C22 C23 1.418(6) . ? C22 H22 0.9300 . ? C23 C24 1.408(6) . ? C23 C28 1.508(6) . ? C24 C25 1.397(6) . ? C24 H24 0.9300 . ? C25 C26 1.413(6) . ? C25 C29 1.525(6) . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C32 1.411(6) . ? C31 C36 1.432(6) . ? C31 C37 1.493(6) . ? C32 C33 1.417(6) . ? C32 H32 0.9300 . ? C33 C34 1.403(6) . ? C33 C38 1.513(6) . ? C34 C35 1.417(6) . ? C34 H34 0.9300 . ? C35 C36 1.405(6) . ? C35 C39 1.512(6) . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? Cr3 C46 2.135(5) . ? Cr3 C42 2.136(5) . ? Cr3 C56 2.144(5) . ? Cr3 C52 2.148(5) . ? Cr3 C41 2.148(5) . ? Cr3 C44 2.154(5) . ? Cr3 C54 2.158(5) . ? Cr3 C45 2.160(5) . ? Cr3 C51 2.163(5) . ? Cr3 C55 2.170(5) . ? Cr3 C53 2.180(5) . ? Cr3 C43 2.180(4) . ? C41 C46 1.427(8) . ? C41 C42 1.436(7) . ? C41 C47 1.495(7) . ? C42 C43 1.390(6) . ? C42 H42 0.9300 . ? C43 C44 1.419(6) . ? C43 C48 1.501(6) . ? C44 C45 1.391(7) . ? C44 H44 0.9300 . ? C45 C46 1.380(8) . ? C45 C49 1.538(7) . ? C46 H46 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C51 C56 1.410(7) . ? C51 C52 1.411(7) . ? C51 C57 1.525(7) . ? C52 C53 1.419(6) . ? C52 H52 0.9300 . ? C53 C54 1.407(7) . ? C53 C58 1.500(6) . ? C54 C55 1.408(7) . ? C54 H54 0.9300 . ? C55 C56 1.423(8) . ? C55 C59 1.488(7) . ? C56 H56 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? Cr4 C72 2.121(5) . ? Cr4 C64 2.133(5) . ? Cr4 C76 2.134(5) . ? Cr4 C73 2.135(5) . ? Cr4 C74 2.144(5) . ? Cr4 C66 2.145(5) . ? Cr4 C62 2.148(5) . ? Cr4 C61 2.161(5) . ? Cr4 C75 2.163(5) . ? Cr4 C65 2.171(5) . ? Cr4 C63 2.173(5) . ? Cr4 C71 2.178(5) . ? C61 C62 1.398(7) . ? C61 C66 1.417(7) . ? C61 C67 1.502(7) . ? C62 C63 1.411(6) . ? C62 H62 0.9300 . ? C63 C64 1.409(7) . ? C63 C68 1.525(7) . ? C64 C65 1.405(7) . ? C64 H64 0.9300 . ? C65 C66 1.424(7) . ? C65 C69 1.514(7) . ? C66 H66 0.9300 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C71 C76 1.402(7) . ? C71 C72 1.406(8) . ? C71 C77 1.527(8) . ? C72 C73 1.395(8) . ? C72 H72 0.9300 . ? C73 C74 1.435(7) . ? C73 C78 1.528(8) . ? C74 C75 1.430(7) . ? C74 H74 0.9300 . ? C75 C76 1.385(7) . ? C75 C79 1.505(7) . ? C76 H76 0.9300 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? O10 C115 1.241(6) . ? O11 C115 1.357(6) . ? O11 C120 1.444(5) . ? O12 C116 1.198(5) . ? O13 C116 1.337(5) . ? O13 C121 1.457(5) . ? O14 C117 1.196(5) . ? O15 C117 1.342(5) . ? O15 C122 1.443(6) . ? O16 C118 1.217(10) . ? O17 C118 1.293(10) . ? O17 C123 1.640(9) . ? O18 C119 1.209(6) . ? O19 C119 1.307(6) . ? O19 C124 1.475(6) . ? C110 C111 1.429(6) . ? C110 C115 1.437(7) . ? C110 C114 1.438(6) . ? C111 C112 1.391(6) . ? C111 C116 1.488(6) . ? C112 C113 1.409(6) . ? C112 C117 1.473(6) . ? C113 C114 1.387(7) . ? C113 C118 1.487(8) . ? C114 C119 1.478(7) . ? C120 H12A 0.9600 . ? C120 H12B 0.9600 . ? C120 H12C 0.9600 . ? C121 H12D 0.9600 . ? C121 H12E 0.9600 . ? C121 H12F 0.9600 . ? C122 H12G 0.9600 . ? C122 H12H 0.9600 . ? C122 H12I 0.9600 . ? C123 H12J 0.9600 . ? C123 H12K 0.9600 . ? C123 H12L 0.9600 . ? C124 H12M 0.9600 . ? C124 H12N 0.9600 . ? C124 H12O 0.9600 . ? O20 C135 1.218(5) . ? O21 C135 1.364(5) . ? O21 C140 1.436(5) . ? O22 C136 1.198(5) . ? O23 C136 1.353(5) . ? O23 C141 1.436(5) . ? O24 C137 1.210(5) . ? O25 C137 1.325(5) . ? O25 C142 1.461(5) . ? O26 C138 1.208(5) . ? O27 C138 1.341(5) . ? O27 C143 1.436(5) . ? O28 C139 1.195(5) . ? O29 C139 1.343(5) . ? O29 C144 1.448(5) . ? C130 C134 1.408(6) . ? C130 C131 1.425(6) . ? C130 C135 1.452(6) . ? C131 C132 1.393(6) . ? C131 C136 1.469(6) . ? C132 C133 1.429(6) . ? C132 C137 1.472(6) . ? C134 C133 1.399(6) . ? C134 C139 1.500(6) . ? C133 C138 1.463(6) . ? C140 H14A 0.9600 . ? C140 H14B 0.9600 . ? C140 H14C 0.9600 . ? C141 H14D 0.9600 . ? C141 H14E 0.9600 . ? C141 H14F 0.9600 . ? C142 H14G 0.9600 . ? C142 H14H 0.9600 . ? C142 H14I 0.9600 . ? C143 H14J 0.9600 . ? C143 H14K 0.9600 . ? C143 H14L 0.9600 . ? C144 H14M 0.9600 . ? C144 H14N 0.9600 . ? C144 H14O 0.9600 . ? O30 C155 1.198(6) . ? O31 C155 1.338(5) . ? O31 C160 1.446(6) . ? O32 C156 1.195(6) . ? O33 C156 1.333(6) . ? O33 C161 1.463(8) . ? O34 C157 1.201(5) . ? O35 C157 1.338(5) . ? O35 C162 1.438(5) . ? O36 C158 1.194(5) . ? O37 C158 1.349(5) . ? O37 C163 1.459(5) . ? O38 C159 1.207(5) . ? O39 C159 1.327(5) . ? O39 C164 1.462(6) . ? C150 C154 1.419(6) . ? C150 C151 1.425(6) . ? C150 C155 1.459(6) . ? C151 C152 1.401(6) . ? C151 C156 1.475(6) . ? C152 C153 1.418(6) . ? C152 C157 1.476(6) . ? C153 C154 1.401(6) . ? C153 C158 1.465(6) . ? C154 C159 1.480(6) . ? C160 H16A 0.9600 . ? C160 H16B 0.9600 . ? C160 H16C 0.9600 . ? C161 H16D 0.9600 . ? C161 H16E 0.9600 . ? C161 H16F 0.9600 . ? C162 H16G 0.9600 . ? C162 H16H 0.9600 . ? C162 H16I 0.9600 . ? C163 H16J 0.9600 . ? C163 H16K 0.9600 . ? C163 H16L 0.9600 . ? C164 H16M 0.9600 . ? C164 H16N 0.9600 . ? C164 H16O 0.9600 . ? O40 C175 1.196(5) . ? O41 C175 1.330(5) . ? O41 C180 1.445(6) . ? O42 C176 1.189(5) . ? O43 C176 1.346(5) . ? O43 C181 1.435(5) . ? O44 C177 1.195(5) . ? O45 C177 1.343(5) . ? O45 C182 1.445(5) . ? O46 C178 1.215(6) . ? O47 C178 1.342(6) . ? O47 C183 1.452(6) . ? O48 C179 1.189(5) . ? O49 C179 1.346(6) . ? O49 C184 1.451(6) . ? C170 C174 1.396(6) . ? C170 C171 1.431(6) . ? C170 C175 1.499(6) . ? C171 C172 1.404(6) . ? C171 C176 1.463(6) . ? C172 C173 1.408(6) . ? C172 C177 1.488(6) . ? C173 C174 1.401(6) . ? C173 C178 1.466(6) . ? C174 C179 1.488(6) . ? C180 H18D 0.9600 . ? C180 H18E 0.9600 . ? C180 H18F 0.9600 . ? C181 H18G 0.9600 . ? C181 H18H 0.9600 . ? C181 H18I 0.9600 . ? C182 H18J 0.9600 . ? C182 H18K 0.9600 . ? C182 H18L 0.9600 . ? C183 H18M 0.9600 . ? C183 H18N 0.9600 . ? C183 H18O 0.9600 . ? C184 H18P 0.9600 . ? C184 H18Q 0.9600 . ? C184 H18R 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Cr1 C14 68.3(2) . . ? C16 Cr1 C6 99.68(18) . . ? C14 Cr1 C6 156.6(2) . . ? C16 Cr1 C12 68.94(19) . . ? C14 Cr1 C12 69.1(2) . . ? C6 Cr1 C12 126.9(2) . . ? C16 Cr1 C2 156.28(19) . . ? C14 Cr1 C2 129.3(2) . . ? C6 Cr1 C2 69.02(18) . . ? C12 Cr1 C2 100.49(19) . . ? C16 Cr1 C4 127.98(19) . . ? C14 Cr1 C4 102.1(2) . . ? C6 Cr1 C4 68.72(18) . . ? C12 Cr1 C4 157.9(2) . . ? C2 Cr1 C4 68.80(18) . . ? C16 Cr1 C15 37.9(2) . . ? C14 Cr1 C15 37.8(2) . . ? C6 Cr1 C15 121.4(2) . . ? C12 Cr1 C15 81.8(2) . . ? C2 Cr1 C15 165.2(2) . . ? C4 Cr1 C15 103.85(19) . . ? C16 Cr1 C13 81.6(2) . . ? C14 Cr1 C13 38.2(3) . . ? C6 Cr1 C13 163.9(3) . . ? C12 Cr1 C13 38.5(2) . . ? C2 Cr1 C13 103.6(2) . . ? C4 Cr1 C13 123.1(2) . . ? C15 Cr1 C13 69.0(3) . . ? C16 Cr1 C3 164.57(19) . . ? C14 Cr1 C3 104.7(2) . . ? C6 Cr1 C3 81.67(17) . . ? C12 Cr1 C3 122.51(19) . . ? C2 Cr1 C3 38.06(17) . . ? C4 Cr1 C3 38.20(17) . . ? C15 Cr1 C3 129.0(2) . . ? C13 Cr1 C3 101.45(19) . . ? C16 Cr1 C11 38.15(18) . . ? C14 Cr1 C11 81.3(2) . . ? C6 Cr1 C11 101.81(18) . . ? C12 Cr1 C11 38.2(2) . . ? C2 Cr1 C11 121.58(19) . . ? C4 Cr1 C11 163.53(19) . . ? C15 Cr1 C11 68.85(19) . . ? C13 Cr1 C11 69.2(2) . . ? C3 Cr1 C11 156.87(19) . . ? C16 Cr1 C5 102.06(18) . . ? C14 Cr1 C5 122.1(2) . . ? C6 Cr1 C5 38.36(18) . . ? C12 Cr1 C5 163.0(2) . . ? C2 Cr1 C5 82.17(18) . . ? C4 Cr1 C5 38.20(17) . . ? C15 Cr1 C5 100.0(2) . . ? C13 Cr1 C5 157.3(2) . . ? C3 Cr1 C5 69.42(17) . . ? C11 Cr1 C5 126.70(19) . . ? C16 Cr1 C1 120.94(18) . . ? C14 Cr1 C1 165.2(2) . . ? C6 Cr1 C1 37.99(18) . . ? C12 Cr1 C1 102.3(2) . . ? C2 Cr1 C1 38.45(17) . . ? C4 Cr1 C1 81.47(18) . . ? C15 Cr1 C1 155.7(2) . . ? C13 Cr1 C1 128.2(3) . . ? C3 Cr1 C1 69.14(17) . . ? C11 Cr1 C1 99.39(18) . . ? C5 Cr1 C1 69.29(19) . . ? C6 C1 C2 118.1(4) . . ? C6 C1 C7 122.0(4) . . ? C2 C1 C7 119.9(4) . . ? C6 C1 Cr1 69.5(3) . . ? C2 C1 Cr1 69.5(3) . . ? C7 C1 Cr1 131.2(4) . . ? C3 C2 C1 121.2(4) . . ? C3 C2 Cr1 71.8(3) . . ? C1 C2 Cr1 72.1(3) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? Cr1 C2 H2 129.2 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 C8 121.6(4) . . ? C4 C3 C8 119.5(4) . . ? C2 C3 Cr1 70.1(3) . . ? C4 C3 Cr1 70.5(3) . . ? C8 C3 Cr1 132.2(3) . . ? C3 C4 C5 121.6(4) . . ? C3 C4 Cr1 71.3(3) . . ? C5 C4 Cr1 71.5(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? Cr1 C4 H4 130.7 . . ? C4 C5 C6 117.7(4) . . ? C4 C5 C9 121.4(4) . . ? C6 C5 C9 120.9(4) . . ? C4 C5 Cr1 70.3(3) . . ? C6 C5 Cr1 69.6(3) . . ? C9 C5 Cr1 131.5(4) . . ? C1 C6 C5 122.4(4) . . ? C1 C6 Cr1 72.5(3) . . ? C5 C6 Cr1 72.1(3) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? Cr1 C6 H6 129.1 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C11 C12 118.4(5) . . ? C16 C11 C17 120.9(5) . . ? C12 C11 C17 120.6(5) . . ? C16 C11 Cr1 69.5(3) . . ? C12 C11 Cr1 69.8(3) . . ? C17 C11 Cr1 130.1(4) . . ? C11 C12 C13 120.7(5) . . ? C11 C12 Cr1 72.0(3) . . ? C13 C12 Cr1 71.4(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? Cr1 C12 H12 129.4 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 C18 120.4(7) . . ? C12 C13 C18 121.1(8) . . ? C14 C13 Cr1 70.1(3) . . ? C12 C13 Cr1 70.1(3) . . ? C18 C13 Cr1 130.1(5) . . ? C15 C14 C13 121.6(5) . . ? C15 C14 Cr1 71.7(3) . . ? C13 C14 Cr1 71.7(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? Cr1 C14 H14 130.0 . . ? C16 C15 C14 118.9(5) . . ? C16 C15 C19 119.5(6) . . ? C14 C15 C19 121.6(6) . . ? C16 C15 Cr1 70.2(3) . . ? C14 C15 Cr1 70.4(4) . . ? C19 C15 Cr1 130.8(4) . . ? C15 C16 C11 121.9(5) . . ? C15 C16 Cr1 72.0(3) . . ? C11 C16 Cr1 72.3(3) . . ? C15 C16 H16 119.1 . . ? C11 C16 H16 119.1 . . ? Cr1 C16 H16 129.1 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C32 Cr2 C24 148.00(17) . . ? C32 Cr2 C36 69.00(16) . . ? C24 Cr2 C36 135.28(17) . . ? C32 Cr2 C22 99.48(16) . . ? C24 Cr2 C22 68.81(16) . . ? C36 Cr2 C22 148.77(17) . . ? C32 Cr2 C34 68.51(16) . . ? C24 Cr2 C34 98.57(16) . . ? C36 Cr2 C34 68.62(16) . . ? C22 Cr2 C34 135.87(16) . . ? C32 Cr2 C31 38.27(16) . . ? C24 Cr2 C31 173.28(18) . . ? C36 Cr2 C31 38.79(16) . . ? C22 Cr2 C31 115.35(16) . . ? C34 Cr2 C31 82.02(16) . . ? C32 Cr2 C26 136.73(16) . . ? C24 Cr2 C26 68.53(16) . . ? C36 Cr2 C26 99.19(17) . . ? C22 Cr2 C26 68.72(16) . . ? C34 Cr2 C26 147.80(16) . . ? C31 Cr2 C26 107.51(16) . . ? C32 Cr2 C33 38.42(16) . . ? C24 Cr2 C33 114.62(17) . . ? C36 Cr2 C33 81.98(16) . . ? C22 Cr2 C33 107.39(16) . . ? C34 Cr2 C33 37.87(16) . . ? C31 Cr2 C33 69.83(16) . . ? C26 Cr2 C33 174.16(17) . . ? C32 Cr2 C25 173.96(18) . . ? C24 Cr2 C25 37.80(17) . . ? C36 Cr2 C25 107.23(17) . . ? C22 Cr2 C25 81.38(16) . . ? C34 Cr2 C25 115.00(16) . . ? C31 Cr2 C25 136.07(18) . . ? C26 Cr2 C25 38.06(16) . . ? C33 Cr2 C25 147.03(17) . . ? C32 Cr2 C35 81.68(16) . . ? C24 Cr2 C35 106.62(16) . . ? C36 Cr2 C35 37.98(17) . . ? C22 Cr2 C35 173.02(17) . . ? C34 Cr2 C35 38.23(16) . . ? C31 Cr2 C35 69.73(16) . . ? C26 Cr2 C35 115.10(16) . . ? C33 Cr2 C35 69.26(16) . . ? C25 Cr2 C35 98.20(15) . . ? C32 Cr2 C23 115.56(16) . . ? C24 Cr2 C23 38.08(17) . . ? C36 Cr2 C23 172.47(17) . . ? C22 Cr2 C23 38.33(15) . . ? C34 Cr2 C23 106.86(16) . . ? C31 Cr2 C23 148.12(17) . . ? C26 Cr2 C23 81.51(16) . . ? C33 Cr2 C23 98.08(16) . . ? C25 Cr2 C23 68.74(17) . . ? C35 Cr2 C23 135.09(17) . . ? C32 Cr2 C21 108.10(15) . . ? C24 Cr2 C21 81.53(15) . . ? C36 Cr2 C21 115.78(16) . . ? C22 Cr2 C21 38.23(15) . . ? C34 Cr2 C21 173.57(17) . . ? C31 Cr2 C21 98.65(16) . . ? C26 Cr2 C21 38.04(16) . . ? C33 Cr2 C21 136.42(16) . . ? C25 Cr2 C21 68.89(16) . . ? C35 Cr2 C21 147.90(17) . . ? C23 Cr2 C21 69.27(16) . . ? C26 C21 C22 118.4(4) . . ? C26 C21 C27 120.7(4) . . ? C22 C21 C27 120.9(4) . . ? C26 C21 Cr2 70.4(2) . . ? C22 C21 Cr2 69.7(2) . . ? C27 C21 Cr2 133.6(3) . . ? C21 C22 C23 121.4(4) . . ? C21 C22 Cr2 72.1(2) . . ? C23 C22 Cr2 71.7(2) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? Cr2 C22 H22 129.5 . . ? C24 C23 C22 118.3(4) . . ? C24 C23 C28 121.2(4) . . ? C22 C23 C28 120.4(4) . . ? C24 C23 Cr2 70.0(2) . . ? C22 C23 Cr2 70.0(2) . . ? C28 C23 Cr2 132.0(3) . . ? C25 C24 C23 121.6(4) . . ? C25 C24 Cr2 72.0(3) . . ? C23 C24 Cr2 71.9(2) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? Cr2 C24 H24 129.4 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 C29 121.9(4) . . ? C26 C25 C29 118.7(4) . . ? C24 C25 Cr2 70.2(2) . . ? C26 C25 Cr2 70.9(2) . . ? C29 C25 Cr2 131.4(3) . . ? C25 C26 C21 120.8(4) . . ? C25 C26 Cr2 71.1(2) . . ? C21 C26 Cr2 71.5(2) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? Cr2 C26 H26 130.4 . . ? C21 C27 H27A 109.5 . . ? C21 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C21 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C31 C36 117.4(4) . . ? C32 C31 C37 121.7(4) . . ? C36 C31 C37 121.0(4) . . ? C32 C31 Cr2 69.9(2) . . ? C36 C31 Cr2 70.0(2) . . ? C37 C31 Cr2 131.9(3) . . ? C31 C32 C33 122.5(4) . . ? C31 C32 Cr2 71.8(2) . . ? C33 C32 Cr2 71.8(2) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? Cr2 C32 H32 130.4 . . ? C34 C33 C32 118.1(4) . . ? C34 C33 C38 120.7(4) . . ? C32 C33 C38 121.1(4) . . ? C34 C33 Cr2 70.7(2) . . ? C32 C33 Cr2 69.8(2) . . ? C38 C33 Cr2 132.1(3) . . ? C33 C34 C35 121.8(4) . . ? C33 C34 Cr2 71.4(2) . . ? C35 C34 Cr2 71.3(2) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? Cr2 C34 H34 131.1 . . ? C36 C35 C34 118.7(4) . . ? C36 C35 C39 121.5(4) . . ? C34 C35 C39 119.8(4) . . ? C36 C35 Cr2 70.2(2) . . ? C34 C35 Cr2 70.5(2) . . ? C39 C35 Cr2 132.1(3) . . ? C35 C36 C31 121.6(4) . . ? C35 C36 Cr2 71.8(2) . . ? C31 C36 Cr2 71.2(2) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? Cr2 C36 H36 130.6 . . ? C31 C37 H37A 109.5 . . ? C31 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C31 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C46 Cr3 C42 70.0(2) . . ? C46 Cr3 C56 99.01(19) . . ? C42 Cr3 C56 140.5(2) . . ? C46 Cr3 C52 145.6(2) . . ? C42 Cr3 C52 98.30(19) . . ? C56 Cr3 C52 69.00(19) . . ? C46 Cr3 C41 38.9(2) . . ? C42 Cr3 C41 39.16(19) . . ? C56 Cr3 C41 109.64(19) . . ? C52 Cr3 C41 112.8(2) . . ? C46 Cr3 C44 67.7(2) . . ? C42 Cr3 C44 68.86(18) . . ? C56 Cr3 C44 143.6(2) . . ? C52 Cr3 C44 139.84(18) . . ? C41 Cr3 C44 81.69(19) . . ? C46 Cr3 C54 138.8(2) . . ? C42 Cr3 C54 143.25(19) . . ? C56 Cr3 C54 68.7(2) . . ? C52 Cr3 C54 68.66(19) . . ? C41 Cr3 C54 177.4(2) . . ? C44 Cr3 C54 98.5(2) . . ? C46 Cr3 C45 37.5(2) . . ? C42 Cr3 C45 82.33(19) . . ? C56 Cr3 C45 112.4(2) . . ? C52 Cr3 C45 176.9(2) . . ? C41 Cr3 C45 69.5(2) . . ? C44 Cr3 C45 37.62(19) . . ? C54 Cr3 C45 109.0(2) . . ? C46 Cr3 C51 113.8(2) . . ? C42 Cr3 C51 110.03(19) . . ? C56 Cr3 C51 38.20(19) . . ? C52 Cr3 C51 38.20(17) . . ? C41 Cr3 C51 98.54(19) . . ? C44 Cr3 C51 177.92(19) . . ? C54 Cr3 C51 81.39(19) . . ? C45 Cr3 C51 144.37(19) . . ? C46 Cr3 C55 109.1(2) . . ? C42 Cr3 C55 178.8(2) . . ? C56 Cr3 C55 38.5(2) . . ? C52 Cr3 C55 81.98(19) . . ? C41 Cr3 C55 139.6(2) . . ? C44 Cr3 C55 111.7(2) . . ? C54 Cr3 C55 37.98(19) . . ? C45 Cr3 C55 97.5(2) . . ? C51 Cr3 C55 69.4(2) . . ? C46 Cr3 C53 176.0(2) . . ? C42 Cr3 C53 111.97(18) . . ? C56 Cr3 C53 81.67(18) . . ? C52 Cr3 C53 38.27(17) . . ? C41 Cr3 C53 144.5(2) . . ? C44 Cr3 C53 109.52(19) . . ? C54 Cr3 C53 37.85(18) . . ? C45 Cr3 C53 138.7(2) . . ? C51 Cr3 C53 69.11(18) . . ? C55 Cr3 C53 68.99(19) . . ? C46 Cr3 C43 80.93(19) . . ? C42 Cr3 C43 37.56(17) . . ? C56 Cr3 C43 177.9(2) . . ? C52 Cr3 C43 109.90(17) . . ? C41 Cr3 C43 69.01(18) . . ? C44 Cr3 C43 38.23(16) . . ? C54 Cr3 C43 112.67(19) . . ? C45 Cr3 C43 68.78(18) . . ? C51 Cr3 C43 139.96(18) . . ? C55 Cr3 C43 143.5(2) . . ? C53 Cr3 C43 98.54(18) . . ? C46 C41 C42 117.6(5) . . ? C46 C41 C47 122.3(5) . . ? C42 C41 C47 120.1(5) . . ? C46 C41 Cr3 70.0(3) . . ? C42 C41 Cr3 70.0(3) . . ? C47 C41 Cr3 132.6(4) . . ? C43 C42 C41 120.4(4) . . ? C43 C42 Cr3 73.0(3) . . ? C41 C42 Cr3 70.9(3) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? Cr3 C42 H42 128.6 . . ? C42 C43 C44 119.4(4) . . ? C42 C43 C48 121.9(4) . . ? C44 C43 C48 118.7(4) . . ? C42 C43 Cr3 69.5(3) . . ? C44 C43 Cr3 69.9(3) . . ? C48 C43 Cr3 131.6(4) . . ? C45 C44 C43 121.5(5) . . ? C45 C44 Cr3 71.5(3) . . ? C43 C44 Cr3 71.9(3) . . ? C45 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? Cr3 C44 H44 130.0 . . ? C46 C45 C44 119.0(5) . . ? C46 C45 C49 121.5(5) . . ? C44 C45 C49 119.5(5) . . ? C46 C45 Cr3 70.3(3) . . ? C44 C45 Cr3 70.9(3) . . ? C49 C45 Cr3 131.1(4) . . ? C45 C46 C41 122.2(5) . . ? C45 C46 Cr3 72.3(3) . . ? C41 C46 Cr3 71.1(3) . . ? C45 C46 H46 118.9 . . ? C41 C46 H46 118.9 . . ? Cr3 C46 H46 130.6 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 119.0(5) . . ? C56 C51 C57 120.0(5) . . ? C52 C51 C57 121.0(5) . . ? C56 C51 Cr3 70.2(3) . . ? C52 C51 Cr3 70.3(3) . . ? C57 C51 Cr3 131.4(4) . . ? C51 C52 C53 121.0(4) . . ? C51 C52 Cr3 71.5(3) . . ? C53 C52 Cr3 72.1(3) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? Cr3 C52 H52 129.4 . . ? C54 C53 C52 118.5(4) . . ? C54 C53 C58 121.4(4) . . ? C52 C53 C58 120.1(4) . . ? C54 C53 Cr3 70.2(3) . . ? C52 C53 Cr3 69.6(3) . . ? C58 C53 Cr3 132.2(4) . . ? C53 C54 C55 122.1(5) . . ? C53 C54 Cr3 71.9(3) . . ? C55 C54 Cr3 71.5(3) . . ? C53 C54 H54 119.0 . . ? C55 C54 H54 119.0 . . ? Cr3 C54 H54 130.5 . . ? C54 C55 C56 118.1(5) . . ? C54 C55 C59 122.6(5) . . ? C56 C55 C59 119.2(5) . . ? C54 C55 Cr3 70.5(3) . . ? C56 C55 Cr3 69.7(3) . . ? C59 C55 Cr3 133.3(4) . . ? C51 C56 C55 121.2(5) . . ? C51 C56 Cr3 71.6(3) . . ? C55 C56 Cr3 71.7(3) . . ? C51 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? Cr3 C56 H56 129.8 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C72 Cr4 C64 153.8(2) . . ? C72 Cr4 C76 68.6(2) . . ? C64 Cr4 C76 132.0(2) . . ? C72 Cr4 C73 38.3(2) . . ? C64 Cr4 C73 119.9(2) . . ? C76 Cr4 C73 82.0(2) . . ? C72 Cr4 C74 69.7(2) . . ? C64 Cr4 C74 100.26(19) . . ? C76 Cr4 C74 69.1(2) . . ? C73 Cr4 C74 39.2(2) . . ? C72 Cr4 C66 129.7(2) . . ? C64 Cr4 C66 69.01(19) . . ? C76 Cr4 C66 99.9(2) . . ? C73 Cr4 C66 166.2(2) . . ? C74 Cr4 C66 154.0(2) . . ? C72 Cr4 C62 98.8(2) . . ? C64 Cr4 C62 68.93(18) . . ? C76 Cr4 C62 152.46(18) . . ? C73 Cr4 C62 103.53(19) . . ? C74 Cr4 C62 131.2(2) . . ? C66 Cr4 C62 68.63(19) . . ? C72 Cr4 C61 102.7(2) . . ? C64 Cr4 C61 82.02(18) . . ? C76 Cr4 C61 118.8(2) . . ? C73 Cr4 C61 129.0(2) . . ? C74 Cr4 C61 167.2(2) . . ? C66 Cr4 C61 38.42(18) . . ? C62 Cr4 C61 37.86(18) . . ? C72 Cr4 C75 81.8(2) . . ? C64 Cr4 C75 105.85(18) . . ? C76 Cr4 C75 37.60(19) . . ? C73 Cr4 C75 70.2(2) . . ? C74 Cr4 C75 38.8(2) . . ? C66 Cr4 C75 119.3(2) . . ? C62 Cr4 C75 169.0(2) . . ? C61 Cr4 C75 152.8(2) . . ? C72 Cr4 C65 167.0(2) . . ? C64 Cr4 C65 38.09(19) . . ? C76 Cr4 C65 105.1(2) . . ? C73 Cr4 C65 154.3(2) . . ? C74 Cr4 C65 119.6(2) . . ? C66 Cr4 C65 38.54(19) . . ? C62 Cr4 C65 81.75(19) . . ? C61 Cr4 C65 69.75(19) . . ? C75 Cr4 C65 100.1(2) . . ? C72 Cr4 C63 119.1(2) . . ? C64 Cr4 C63 38.19(17) . . ? C76 Cr4 C63 168.86(18) . . ? C73 Cr4 C63 99.4(2) . . ? C74 Cr4 C63 105.0(2) . . ? C66 Cr4 C63 81.49(19) . . ? C62 Cr4 C63 38.10(16) . . ? C61 Cr4 C63 68.95(18) . . ? C75 Cr4 C63 132.48(19) . . ? C65 Cr4 C63 69.03(19) . . ? C72 Cr4 C71 38.1(2) . . ? C64 Cr4 C71 167.8(2) . . ? C76 Cr4 C71 37.92(19) . . ? C73 Cr4 C71 69.4(2) . . ? C74 Cr4 C71 82.4(2) . . ? C66 Cr4 C71 103.5(2) . . ? C62 Cr4 C71 118.23(19) . . ? C61 Cr4 C71 98.1(2) . . ? C75 Cr4 C71 68.76(19) . . ? C65 Cr4 C71 130.6(2) . . ? C63 Cr4 C71 152.7(2) . . ? C62 C61 C66 118.6(4) . . ? C62 C61 C67 121.3(4) . . ? C66 C61 C67 120.1(4) . . ? C62 C61 Cr4 70.6(3) . . ? C66 C61 Cr4 70.2(3) . . ? C67 C61 Cr4 131.6(4) . . ? C61 C62 C63 121.7(4) . . ? C61 C62 Cr4 71.6(3) . . ? C63 C62 Cr4 71.9(3) . . ? C61 C62 H62 119.1 . . ? C63 C62 H62 119.1 . . ? Cr4 C62 H62 130.0 . . ? C64 C63 C62 118.4(4) . . ? C64 C63 C68 120.2(4) . . ? C62 C63 C68 121.3(4) . . ? C64 C63 Cr4 69.4(3) . . ? C62 C63 Cr4 70.0(3) . . ? C68 C63 Cr4 131.7(4) . . ? C65 C64 C63 122.0(5) . . ? C65 C64 Cr4 72.4(3) . . ? C63 C64 Cr4 72.4(3) . . ? C65 C64 H64 119.0 . . ? C63 C64 H64 119.0 . . ? Cr4 C64 H64 128.5 . . ? C64 C65 C66 117.9(5) . . ? C64 C65 C69 121.7(5) . . ? C66 C65 C69 120.4(5) . . ? C64 C65 Cr4 69.5(3) . . ? C66 C65 Cr4 69.8(3) . . ? C69 C65 Cr4 131.0(4) . . ? C61 C66 C65 121.3(5) . . ? C61 C66 Cr4 71.4(3) . . ? C65 C66 Cr4 71.7(3) . . ? C61 C66 H66 119.3 . . ? C65 C66 H66 119.3 . . ? Cr4 C66 H66 130.2 . . ? C61 C67 H67A 109.5 . . ? C61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C63 C68 H68A 109.5 . . ? C63 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C63 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C65 C69 H69A 109.5 . . ? C65 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C65 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C76 C71 C72 117.2(5) . . ? C76 C71 C77 120.7(6) . . ? C72 C71 C77 122.0(6) . . ? C76 C71 Cr4 69.3(3) . . ? C72 C71 Cr4 68.7(3) . . ? C77 C71 Cr4 130.6(5) . . ? C73 C72 C71 122.6(5) . . ? C73 C72 Cr4 71.4(3) . . ? C71 C72 Cr4 73.1(3) . . ? C73 C72 H72 118.7 . . ? C71 C72 H72 118.7 . . ? Cr4 C72 H72 129.4 . . ? C72 C73 C74 118.8(5) . . ? C72 C73 C78 122.0(5) . . ? C74 C73 C78 119.1(5) . . ? C72 C73 Cr4 70.3(3) . . ? C74 C73 Cr4 70.7(3) . . ? C78 C73 Cr4 129.4(4) . . ? C75 C74 C73 119.2(5) . . ? C75 C74 Cr4 71.3(3) . . ? C73 C74 Cr4 70.1(3) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.4 . . ? Cr4 C74 H74 130.7 . . ? C76 C75 C74 118.9(5) . . ? C76 C75 C79 120.5(5) . . ? C74 C75 C79 120.6(5) . . ? C76 C75 Cr4 70.1(3) . . ? C74 C75 Cr4 69.9(3) . . ? C79 C75 Cr4 132.7(4) . . ? C75 C76 C71 123.2(5) . . ? C75 C76 Cr4 72.3(3) . . ? C71 C76 Cr4 72.7(3) . . ? C75 C76 H76 118.4 . . ? C71 C76 H76 118.4 . . ? Cr4 C76 H76 129.1 . . ? C71 C77 H77A 109.5 . . ? C71 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C71 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C75 C79 H79A 109.5 . . ? C75 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C75 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C115 O11 C120 116.2(4) . . ? C116 O13 C121 115.2(4) . . ? C117 O15 C122 118.9(4) . . ? C118 O17 C123 98.0(7) . . ? C119 O19 C124 113.0(4) . . ? C111 C110 C115 124.2(4) . . ? C111 C110 C114 107.3(4) . . ? C115 C110 C114 128.1(4) . . ? C112 C111 C110 107.4(4) . . ? C112 C111 C116 126.5(4) . . ? C110 C111 C116 126.1(4) . . ? C111 C112 C113 109.0(4) . . ? C111 C112 C117 125.9(4) . . ? C113 C112 C117 125.1(4) . . ? C114 C113 C112 108.8(4) . . ? C114 C113 C118 127.3(5) . . ? C112 C113 C118 123.6(5) . . ? C113 C114 C110 107.4(4) . . ? C113 C114 C119 120.3(4) . . ? C110 C114 C119 132.2(4) . . ? O10 C115 O11 121.4(5) . . ? O10 C115 C110 126.3(5) . . ? O11 C115 C110 112.3(4) . . ? O12 C116 O13 123.4(4) . . ? O12 C116 C111 125.0(4) . . ? O13 C116 C111 111.6(4) . . ? O14 C117 O15 123.2(4) . . ? O14 C117 C112 126.0(4) . . ? O15 C117 C112 110.8(4) . . ? O16 C118 O17 124.0(6) . . ? O16 C118 C113 123.7(8) . . ? O17 C118 C113 112.3(8) . . ? O18 C119 O19 123.3(5) . . ? O18 C119 C114 121.8(5) . . ? O19 C119 C114 114.8(4) . . ? O11 C120 H12A 109.5 . . ? O11 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? O11 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? O13 C121 H12D 109.5 . . ? O13 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? O13 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? O15 C122 H12G 109.5 . . ? O15 C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? O15 C122 H12I 109.5 . . ? H12G C122 H12I 109.5 . . ? H12H C122 H12I 109.5 . . ? O17 C123 H12J 109.5 . . ? O17 C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? O17 C123 H12L 109.5 . . ? H12J C123 H12L 109.5 . . ? H12K C123 H12L 109.5 . . ? O19 C124 H12M 109.5 . . ? O19 C124 H12N 109.5 . . ? H12M C124 H12N 109.5 . . ? O19 C124 H12O 109.5 . . ? H12M C124 H12O 109.5 . . ? H12N C124 H12O 109.5 . . ? C135 O21 C140 116.1(3) . . ? C136 O23 C141 116.0(4) . . ? C137 O25 C142 115.8(4) . . ? C138 O27 C143 115.7(4) . . ? C139 O29 C144 115.3(3) . . ? C134 C130 C131 106.9(4) . . ? C134 C130 C135 125.6(4) . . ? C131 C130 C135 127.5(4) . . ? C132 C131 C130 109.0(4) . . ? C132 C131 C136 122.4(4) . . ? C130 C131 C136 128.3(4) . . ? C131 C132 C133 107.4(4) . . ? C131 C132 C137 127.6(4) . . ? C133 C132 C137 124.8(4) . . ? C133 C134 C130 108.8(4) . . ? C133 C134 C139 124.5(4) . . ? C130 C134 C139 126.5(4) . . ? C134 C133 C132 107.9(4) . . ? C134 C133 C138 128.5(4) . . ? C132 C133 C138 123.3(4) . . ? O20 C135 O21 121.9(4) . . ? O20 C135 C130 127.2(4) . . ? O21 C135 C130 110.9(4) . . ? O22 C136 O23 122.1(4) . . ? O22 C136 C131 126.9(4) . . ? O23 C136 C131 110.9(4) . . ? O24 C137 O25 122.6(4) . . ? O24 C137 C132 124.5(4) . . ? O25 C137 C132 112.9(4) . . ? O26 C138 O27 122.4(4) . . ? O26 C138 C133 124.3(4) . . ? O27 C138 C133 113.2(4) . . ? O28 C139 O29 123.6(4) . . ? O28 C139 C134 124.8(4) . . ? O29 C139 C134 111.6(4) . . ? O21 C140 H14A 109.5 . . ? O21 C140 H14B 109.5 . . ? H14A C140 H14B 109.5 . . ? O21 C140 H14C 109.5 . . ? H14A C140 H14C 109.5 . . ? H14B C140 H14C 109.5 . . ? O23 C141 H14D 109.5 . . ? O23 C141 H14E 109.5 . . ? H14D C141 H14E 109.5 . . ? O23 C141 H14F 109.5 . . ? H14D C141 H14F 109.5 . . ? H14E C141 H14F 109.5 . . ? O25 C142 H14G 109.5 . . ? O25 C142 H14H 109.5 . . ? H14G C142 H14H 109.5 . . ? O25 C142 H14I 109.5 . . ? H14G C142 H14I 109.5 . . ? H14H C142 H14I 109.5 . . ? O27 C143 H14J 109.5 . . ? O27 C143 H14K 109.5 . . ? H14J C143 H14K 109.5 . . ? O27 C143 H14L 109.5 . . ? H14J C143 H14L 109.5 . . ? H14K C143 H14L 109.5 . . ? O29 C144 H14M 109.5 . . ? O29 C144 H14N 109.5 . . ? H14M C144 H14N 109.5 . . ? O29 C144 H14O 109.5 . . ? H14M C144 H14O 109.5 . . ? H14N C144 H14O 109.5 . . ? C155 O31 C160 115.7(4) . . ? C156 O33 C161 113.7(5) . . ? C157 O35 C162 116.3(4) . . ? C158 O37 C163 115.4(4) . . ? C159 O39 C164 115.1(4) . . ? C154 C150 C151 107.4(4) . . ? C154 C150 C155 127.3(4) . . ? C151 C150 C155 125.2(4) . . ? C152 C151 C150 108.3(4) . . ? C152 C151 C156 124.7(4) . . ? C150 C151 C156 126.8(4) . . ? C151 C152 C153 107.8(4) . . ? C151 C152 C157 124.6(4) . . ? C153 C152 C157 127.6(4) . . ? C154 C153 C152 108.6(4) . . ? C154 C153 C158 126.8(4) . . ? C152 C153 C158 124.5(4) . . ? C153 C154 C150 107.9(4) . . ? C153 C154 C159 125.7(4) . . ? C150 C154 C159 126.2(4) . . ? O30 C155 O31 122.3(4) . . ? O30 C155 C150 126.1(4) . . ? O31 C155 C150 111.6(4) . . ? O32 C156 O33 121.7(5) . . ? O32 C156 C151 126.3(4) . . ? O33 C156 C151 111.9(5) . . ? O34 C157 O35 122.4(4) . . ? O34 C157 C152 125.7(4) . . ? O35 C157 C152 111.9(4) . . ? O36 C158 O37 122.7(4) . . ? O36 C158 C153 125.3(4) . . ? O37 C158 C153 111.9(4) . . ? O38 C159 O39 122.7(4) . . ? O38 C159 C154 123.9(4) . . ? O39 C159 C154 113.4(4) . . ? O31 C160 H16A 109.5 . . ? O31 C160 H16B 109.5 . . ? H16A C160 H16B 109.5 . . ? O31 C160 H16C 109.5 . . ? H16A C160 H16C 109.5 . . ? H16B C160 H16C 109.5 . . ? O33 C161 H16D 109.5 . . ? O33 C161 H16E 109.5 . . ? H16D C161 H16E 109.5 . . ? O33 C161 H16F 109.5 . . ? H16D C161 H16F 109.5 . . ? H16E C161 H16F 109.5 . . ? O35 C162 H16G 109.5 . . ? O35 C162 H16H 109.5 . . ? H16G C162 H16H 109.5 . . ? O35 C162 H16I 109.5 . . ? H16G C162 H16I 109.5 . . ? H16H C162 H16I 109.5 . . ? O37 C163 H16J 109.5 . . ? O37 C163 H16K 109.5 . . ? H16J C163 H16K 109.5 . . ? O37 C163 H16L 109.5 . . ? H16J C163 H16L 109.5 . . ? H16K C163 H16L 109.5 . . ? O39 C164 H16M 109.5 . . ? O39 C164 H16N 109.5 . . ? H16M C164 H16N 109.5 . . ? O39 C164 H16O 109.5 . . ? H16M C164 H16O 109.5 . . ? H16N C164 H16O 109.5 . . ? C175 O41 C180 116.1(4) . . ? C176 O43 C181 116.2(4) . . ? C177 O45 C182 114.7(4) . . ? C178 O47 C183 114.2(5) . . ? C179 O49 C184 114.8(4) . . ? C174 C170 C171 108.6(4) . . ? C174 C170 C175 124.1(4) . . ? C171 C170 C175 127.0(4) . . ? C172 C171 C170 106.7(4) . . ? C172 C171 C176 124.0(4) . . ? C170 C171 C176 129.3(4) . . ? C171 C172 C173 108.4(4) . . ? C171 C172 C177 125.5(4) . . ? C173 C172 C177 126.0(4) . . ? C174 C173 C172 108.5(4) . . ? C174 C173 C178 128.4(4) . . ? C172 C173 C178 123.1(4) . . ? C170 C174 C173 107.8(4) . . ? C170 C174 C179 123.8(4) . . ? C173 C174 C179 128.4(4) . . ? O40 C175 O41 122.8(4) . . ? O40 C175 C170 125.6(4) . . ? O41 C175 C170 111.6(4) . . ? O42 C176 O43 122.7(4) . . ? O42 C176 C171 125.7(4) . . ? O43 C176 C171 111.6(4) . . ? O44 C177 O45 123.0(4) . . ? O44 C177 C172 124.9(4) . . ? O45 C177 C172 112.1(4) . . ? O46 C178 O47 122.4(5) . . ? O46 C178 C173 124.9(5) . . ? O47 C178 C173 112.7(5) . . ? O48 C179 O49 123.1(4) . . ? O48 C179 C174 126.8(4) . . ? O49 C179 C174 110.1(4) . . ? O41 C180 H18D 109.5 . . ? O41 C180 H18E 109.5 . . ? H18D C180 H18E 109.5 . . ? O41 C180 H18F 109.5 . . ? H18D C180 H18F 109.5 . . ? H18E C180 H18F 109.5 . . ? O43 C181 H18G 109.5 . . ? O43 C181 H18H 109.5 . . ? H18G C181 H18H 109.5 . . ? O43 C181 H18I 109.5 . . ? H18G C181 H18I 109.5 . . ? H18H C181 H18I 109.5 . . ? O45 C182 H18J 109.5 . . ? O45 C182 H18K 109.5 . . ? H18J C182 H18K 109.5 . . ? O45 C182 H18L 109.5 . . ? H18J C182 H18L 109.5 . . ? H18K C182 H18L 109.5 . . ? O47 C183 H18M 109.5 . . ? O47 C183 H18N 109.5 . . ? H18M C183 H18N 109.5 . . ? O47 C183 H18O 109.5 . . ? H18M C183 H18O 109.5 . . ? H18N C183 H18O 109.5 . . ? O49 C184 H18P 109.5 . . ? O49 C184 H18Q 109.5 . . ? H18P C184 H18Q 109.5 . . ? O49 C184 H18R 109.5 . . ? H18P C184 H18R 109.5 . . ? H18Q C184 H18R 109.5 . . ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max .702 _refine_diff_density_min -.652 _refine_diff_density_rms .078 # Attachment 'Moisopropyl.cif' data_jul1904 _database_code_depnum_ccdc_archive 'CCDC 607083' _audit_creation_date 2004-07-21T11:34:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H48 Mo, C15 H15 O10, 2(C4 H8 O)' _chemical_formula_sum 'C53 H79 Mo O12' _chemical_formula_weight 1004.1 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6201(5) _cell_length_b 12.7552(5) _cell_length_c 18.5897(7) _cell_angle_alpha 75.820(2) _cell_angle_beta 84.673(2) _cell_angle_gamma 76.999(2) _cell_volume 2600.80(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37528 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1070 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9846 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.379078E-1 _diffrn_orient_matrix_ub_12 -0.254529E-1 _diffrn_orient_matrix_ub_13 0.498718E-1 _diffrn_orient_matrix_ub_21 -0.788037E-1 _diffrn_orient_matrix_ub_22 0.425078E-1 _diffrn_orient_matrix_ub_23 -0.189922E-1 _diffrn_orient_matrix_ub_31 -0.128915E-1 _diffrn_orient_matrix_ub_32 -0.662135E-1 _diffrn_orient_matrix_ub_33 -0.15345E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_unetI/netI 0.0517 _diffrn_reflns_number 33339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.24 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 9150 _reflns_number_gt 6562 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are two poorly defined thf solvate molecules which were included with SADI constraints. The largest areas of residual density are near the solvate molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+7.8721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 9150 _refine_ls_number_parameters 598 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.094 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.706 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0 0.5 0.5 0.02291(17) Uani 1 2 d S . . Mo2 Mo 0.5 0.5 0 0.02322(17) Uani 1 2 d S . . O1 O 0.1780(3) 1.0726(3) 0.55498(19) 0.0394(9) Uani 1 1 d . A 1 O2 O 0.3446(3) 0.9429(3) 0.57809(18) 0.0351(8) Uani 1 1 d . A 1 O3 O 0.4834(3) 1.0677(4) 0.6422(2) 0.0502(10) Uani 1 1 d . A 1 O4 O 0.5310(3) 0.9386(3) 0.7467(2) 0.0439(9) Uani 1 1 d . A 1 O5 O 0.3488(4) 0.9399(4) 0.9223(2) 0.0588(12) Uani 1 1 d . A 1 O6 O 0.4172(3) 1.0762(3) 0.84145(19) 0.0392(9) Uani 1 1 d . A 1 O7 O 0.0738(5) 1.0616(4) 0.9019(2) 0.0687(14) Uani 1 1 d . A 1 O8 O 0.0052(3) 0.9309(3) 0.8689(2) 0.0476(10) Uani 1 1 d . A 1 O9 O -0.0736(3) 1.0456(4) 0.7202(2) 0.0598(12) Uani 1 1 d . A 1 O10 O 0.0296(3) 0.9329(3) 0.6509(2) 0.0426(9) Uani 1 1 d . A 1 C1 C -0.1958(4) 0.5861(4) 0.5092(3) 0.0278(10) Uani 1 1 d . B 1 C2 C -0.1390(4) 0.6525(4) 0.4497(3) 0.0286(11) Uani 1 1 d . B 1 H2 H -0.1419 0.7274 0.4502 0.034 Uiso 1 1 calc R B 1 C3 C -0.0786(4) 0.6101(4) 0.3900(3) 0.0285(11) Uani 1 1 d . B 1 C4 C -0.0740(4) 0.4971(4) 0.3914(3) 0.0285(11) Uani 1 1 d . B 1 H4 H -0.0322 0.467 0.3522 0.034 Uiso 1 1 calc R B 1 C5 C -0.1295(4) 0.4278(4) 0.4494(3) 0.0289(11) Uani 1 1 d . B 1 C6 C -0.1885(4) 0.4735(4) 0.5075(3) 0.0279(10) Uani 1 1 d . B 1 H6 H -0.2249 0.428 0.5472 0.033 Uiso 1 1 calc R B 1 C7 C -0.2711(4) 0.6340(4) 0.5696(3) 0.0352(12) Uani 1 1 d . B 1 H7 H -0.2807 0.5715 0.6126 0.042 Uiso 1 1 calc R B 1 C8 C -0.2184(5) 0.7154(4) 0.5975(3) 0.0408(13) Uani 1 1 d . B 1 H8A H -0.2714 0.7426 0.6362 0.061 Uiso 1 1 calc R B 1 H8B H -0.2089 0.7779 0.5562 0.061 Uiso 1 1 calc R B 1 H8C H -0.1412 0.6781 0.6181 0.061 Uiso 1 1 calc R B 1 C9 C -0.3935(5) 0.6903(6) 0.5391(4) 0.0614(18) Uani 1 1 d . B 1 H9A H -0.4439 0.7213 0.5773 0.092 Uiso 1 1 calc R B 1 H9B H -0.4293 0.6357 0.5253 0.092 Uiso 1 1 calc R B 1 H9C H -0.3857 0.7497 0.4953 0.092 Uiso 1 1 calc R B 1 C10 C -0.0311(5) 0.6856(4) 0.3232(3) 0.0361(12) Uani 1 1 d . B 1 H10 H -0.0232 0.7533 0.3387 0.043 Uiso 1 1 calc R B 1 C11 C -0.1230(5) 0.7214(5) 0.2630(3) 0.0487(15) Uani 1 1 d . B 1 H11A H -0.094 0.7705 0.2193 0.073 Uiso 1 1 calc R B 1 H11B H -0.1974 0.7606 0.2822 0.073 Uiso 1 1 calc R B 1 H11C H -0.1364 0.6559 0.2491 0.073 Uiso 1 1 calc R B 1 C12 C 0.0891(5) 0.6355(5) 0.2924(3) 0.0559(17) Uani 1 1 d . B 1 H12A H 0.1136 0.6894 0.2498 0.084 Uiso 1 1 calc R B 1 H12B H 0.0839 0.5689 0.2767 0.084 Uiso 1 1 calc R B 1 H12C H 0.1473 0.6161 0.331 0.084 Uiso 1 1 calc R B 1 C13 C -0.1330(5) 0.3122(4) 0.4435(3) 0.0343(12) Uani 1 1 d . B 1 H13 H -0.0657 0.2889 0.4093 0.041 Uiso 1 1 calc R B 1 C14 C -0.1200(5) 0.2257(4) 0.5161(3) 0.0443(14) Uani 1 1 d . B 1 H14A H -0.1232 0.1538 0.5072 0.066 Uiso 1 1 calc R B 1 H14B H -0.1845 0.2465 0.5512 0.066 Uiso 1 1 calc R B 1 H14C H -0.0441 0.2208 0.537 0.066 Uiso 1 1 calc R B 1 C15 C -0.2469(6) 0.3159(5) 0.4074(4) 0.0590(18) Uani 1 1 d . B 1 H15A H -0.2496 0.2414 0.4033 0.088 Uiso 1 1 calc R B 1 H15B H -0.2494 0.3653 0.3578 0.088 Uiso 1 1 calc R B 1 H15C H -0.315 0.3434 0.438 0.088 Uiso 1 1 calc R B 1 C16 C 0.6415(4) 0.5661(4) 0.0444(3) 0.0283(11) Uani 1 1 d . C 1 C17 C 0.6947(4) 0.5110(4) -0.0121(3) 0.0283(10) Uani 1 1 d . C 1 H17 H 0.7342 0.5504 -0.0534 0.034 Uiso 1 1 calc R C 1 C18 C 0.6911(4) 0.3998(4) -0.0089(3) 0.0270(10) Uani 1 1 d . C 1 C19 C 0.6312(4) 0.3429(4) 0.0535(2) 0.0259(10) Uani 1 1 d . C 1 H19 H 0.6275 0.2682 0.0566 0.031 Uiso 1 1 calc R C 1 C20 C 0.5771(4) 0.3938(4) 0.1110(2) 0.0281(11) Uani 1 1 d . C 1 C21 C 0.5815(4) 0.5058(4) 0.1054(3) 0.0281(10) Uani 1 1 d . C 1 H21 H 0.5436 0.5414 0.1432 0.034 Uiso 1 1 calc R C 1 C22 C 0.6543(5) 0.6824(4) 0.0435(3) 0.0374(12) Uani 1 1 d . C 1 H22 H 0.5867 0.7153 0.074 0.045 Uiso 1 1 calc R C 1 C23 C 0.6524(5) 0.7590(5) -0.0332(3) 0.0486(15) Uani 1 1 d . C 1 H23A H 0.6606 0.8321 -0.0291 0.073 Uiso 1 1 calc R C 1 H23B H 0.5773 0.7658 -0.0558 0.073 Uiso 1 1 calc R C 1 H23C H 0.718 0.7287 -0.0643 0.073 Uiso 1 1 calc R C 1 C24 C 0.7681(6) 0.6762(5) 0.0806(4) 0.0584(17) Uani 1 1 d . C 1 H24A H 0.7763 0.7511 0.0804 0.088 Uiso 1 1 calc R C 1 H24B H 0.8358 0.6407 0.0532 0.088 Uiso 1 1 calc R C 1 H24C H 0.7654 0.6329 0.1319 0.088 Uiso 1 1 calc R C 1 C25 C 0.7597(4) 0.3423(4) -0.0671(3) 0.0334(11) Uani 1 1 d . C 1 H25 H 0.7681 0.4004 -0.1132 0.04 Uiso 1 1 calc R C 1 C26 C 0.8838(5) 0.2874(6) -0.0393(4) 0.0567(17) Uani 1 1 d . C 1 H26A H 0.9298 0.2502 -0.0762 0.085 Uiso 1 1 calc R C 1 H26B H 0.8779 0.2331 0.0077 0.085 Uiso 1 1 calc R C 1 H26C H 0.9231 0.3439 -0.0314 0.085 Uiso 1 1 calc R C 1 C27 C 0.7009(5) 0.2589(5) -0.0874(3) 0.0437(13) Uani 1 1 d . C 1 H27A H 0.75 0.226 -0.1253 0.066 Uiso 1 1 calc R C 1 H27B H 0.623 0.2963 -0.1069 0.066 Uiso 1 1 calc R C 1 H27C H 0.6918 0.2007 -0.0432 0.066 Uiso 1 1 calc R C 1 C28 C 0.5244(4) 0.3261(4) 0.1807(3) 0.0345(12) Uani 1 1 d . C 1 H28 H 0.5071 0.2596 0.168 0.041 Uiso 1 1 calc R C 1 C29 C 0.4103(5) 0.3886(5) 0.2114(3) 0.0527(16) Uani 1 1 d . C 1 H29A H 0.3817 0.3402 0.2556 0.079 Uiso 1 1 calc R C 1 H29B H 0.3504 0.4116 0.1736 0.079 Uiso 1 1 calc R C 1 H29C H 0.4253 0.4539 0.2246 0.079 Uiso 1 1 calc R C 1 C30 C 0.6181(5) 0.2866(4) 0.2393(3) 0.0395(13) Uani 1 1 d . C 1 H30A H 0.6905 0.246 0.219 0.059 Uiso 1 1 calc R C 1 H30B H 0.5889 0.2379 0.2832 0.059 Uiso 1 1 calc R C 1 H30C H 0.6351 0.3506 0.2535 0.059 Uiso 1 1 calc R C 1 C31 C 0.2397(4) 1.0028(4) 0.6792(3) 0.0296(11) Uani 1 1 d . A 1 C32 C 0.3307(4) 1.0035(4) 0.7240(3) 0.0299(11) Uani 1 1 d . A 1 C33 C 0.2834(4) 0.9980(4) 0.7975(3) 0.0318(11) Uani 1 1 d . A 1 C34 C 0.1642(4) 0.9931(4) 0.7982(3) 0.0309(11) Uani 1 1 d . A 1 C35 C 0.1359(4) 0.9962(4) 0.7247(3) 0.0295(11) Uani 1 1 d . A 1 C36 C 0.2485(4) 1.0117(4) 0.5986(3) 0.0290(11) Uani 1 1 d . A 1 C37 C 0.3642(5) 0.9538(5) 0.4990(3) 0.0385(12) Uani 1 1 d . A 1 H37A H 0.4357 0.9007 0.4893 0.058 Uiso 1 1 calc R A 1 H37B H 0.3739 1.029 0.4753 0.058 Uiso 1 1 calc R A 1 H37C H 0.2963 0.9389 0.4786 0.058 Uiso 1 1 calc R A 1 C38 C 0.4528(4) 1.0089(4) 0.6986(3) 0.0335(11) Uani 1 1 d . A 1 C39 C 0.6529(5) 0.9455(6) 0.7302(4) 0.0637(18) Uani 1 1 d . A 1 H39A H 0.7022 0.8916 0.7683 0.096 Uiso 1 1 calc R A 1 H39B H 0.6623 1.0201 0.7296 0.096 Uiso 1 1 calc R A 1 H39C H 0.6773 0.9293 0.6815 0.096 Uiso 1 1 calc R A 1 C40 C 0.3502(5) 0.9987(4) 0.8607(3) 0.0358(12) Uani 1 1 d . A 1 C41 C 0.5049(6) 1.0693(5) 0.8930(3) 0.0516(16) Uani 1 1 d . A 1 H41A H 0.5483 1.1287 0.874 0.077 Uiso 1 1 calc R A 1 H41B H 0.56 0.9975 0.899 0.077 Uiso 1 1 calc R A 1 H41C H 0.4661 1.077 0.9411 0.077 Uiso 1 1 calc R A 1 C42 C 0.0790(5) 0.9996(4) 0.8613(3) 0.0388(12) Uani 1 1 d . A 1 C43 C -0.0957(6) 0.9467(6) 0.9204(4) 0.0655(19) Uani 1 1 d . A 1 H43A H -0.1432 0.8918 0.9217 0.098 Uiso 1 1 calc R A 1 H43B H -0.144 1.0212 0.9041 0.098 Uiso 1 1 calc R A 1 H43C H -0.0679 0.9379 0.9701 0.098 Uiso 1 1 calc R A 1 C44 C 0.0203(4) 0.9961(4) 0.7005(3) 0.0314(11) Uani 1 1 d . A 1 C45 C -0.0769(5) 0.9325(5) 0.6181(3) 0.0488(14) Uani 1 1 d . A 1 H45A H -0.059 0.8836 0.5835 0.073 Uiso 1 1 calc R A 1 H45B H -0.1114 1.0077 0.5912 0.073 Uiso 1 1 calc R A 1 H45C H -0.1333 0.906 0.6571 0.073 Uiso 1 1 calc R A 1 O1S O 0.5833(8) 0.6418(9) 0.3469(5) 0.175(4) Uani 1 1 d D D 1 O2S O 0.0877(7) 0.6516(10) 0.8474(5) 0.172(4) Uani 1 1 d D E 1 C1S C 0.5906(14) 0.6483(14) 0.2700(6) 0.226(10) Uani 1 1 d D D 1 H1S1 H 0.615 0.7178 0.2436 0.271 Uiso 1 1 calc R D 1 H1S2 H 0.6519 0.5858 0.2592 0.271 Uiso 1 1 calc R D 1 C2S C 0.4899(7) 0.6456(8) 0.2454(5) 0.085(2) Uani 1 1 d D D 1 H2S1 H 0.4892 0.5707 0.2396 0.102 Uiso 1 1 calc R D 1 H2S2 H 0.4738 0.6991 0.1971 0.102 Uiso 1 1 calc R D 1 C3S C 0.4035(9) 0.6763(16) 0.3028(9) 0.275(13) Uani 1 1 d D D 1 H3S1 H 0.3753 0.7576 0.2917 0.33 Uiso 1 1 calc R D 1 H3S2 H 0.3346 0.6422 0.3038 0.33 Uiso 1 1 calc R D 1 C4S C 0.4541(14) 0.641(2) 0.3699(7) 0.282(14) Uani 1 1 d D D 1 H4S1 H 0.443 0.5661 0.3952 0.338 Uiso 1 1 calc R D 1 H4S2 H 0.4223 0.6926 0.4025 0.338 Uiso 1 1 calc R D 1 C5S C 0.0680(13) 0.6593(13) 0.7721(5) 0.170(7) Uani 1 1 d D E 1 H5S1 H 0.0837 0.7295 0.7402 0.204 Uiso 1 1 calc R E 1 H5S2 H 0.1191 0.5967 0.7542 0.204 Uiso 1 1 calc R E 1 C6S C -0.0477(13) 0.6556(14) 0.7721(8) 0.313(17) Uani 1 1 d D E 1 H6S1 H -0.0558 0.6073 0.7393 0.376 Uiso 1 1 calc R E 1 H6S2 H -0.0925 0.7309 0.7504 0.376 Uiso 1 1 calc R E 1 C7S C -0.0993(8) 0.6170(9) 0.8421(8) 0.145(6) Uani 1 1 d D E 1 H7S1 H -0.1715 0.6701 0.8527 0.174 Uiso 1 1 calc R E 1 H7S2 H -0.1189 0.5441 0.8463 0.174 Uiso 1 1 calc R E 1 C8S C -0.0161(11) 0.6099(19) 0.8854(8) 0.242(11) Uani 1 1 d D E 1 H8S1 H 0.0103 0.5315 0.9112 0.29 Uiso 1 1 calc R E 1 H8S2 H -0.0486 0.6519 0.9236 0.29 Uiso 1 1 calc R E 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0222(3) 0.0224(3) 0.0242(3) -0.0033(2) -0.0026(2) -0.0066(2) Mo2 0.0198(3) 0.0253(3) 0.0241(3) -0.0035(2) -0.0025(2) -0.0055(2) O1 0.037(2) 0.041(2) 0.035(2) -0.0056(16) -0.0056(17) 0.0019(17) O2 0.0337(19) 0.041(2) 0.0277(17) -0.0111(15) -0.0017(15) 0.0013(16) O3 0.048(2) 0.070(3) 0.035(2) -0.0059(19) 0.0078(18) -0.027(2) O4 0.031(2) 0.049(2) 0.049(2) -0.0102(18) -0.0012(17) -0.0038(17) O5 0.089(3) 0.059(3) 0.030(2) 0.0025(19) -0.009(2) -0.032(2) O6 0.049(2) 0.036(2) 0.0344(19) -0.0071(16) -0.0083(17) -0.0113(17) O7 0.096(4) 0.063(3) 0.056(3) -0.029(2) 0.038(3) -0.035(3) O8 0.041(2) 0.061(3) 0.043(2) -0.0144(19) 0.0173(18) -0.021(2) O9 0.034(2) 0.082(3) 0.067(3) -0.039(2) -0.005(2) 0.006(2) O10 0.030(2) 0.046(2) 0.059(2) -0.0249(19) 0.0007(18) -0.0111(16) C1 0.023(2) 0.027(3) 0.034(3) -0.008(2) -0.005(2) -0.0030(19) C2 0.030(3) 0.025(3) 0.030(3) -0.003(2) -0.007(2) -0.007(2) C3 0.028(3) 0.028(3) 0.030(3) -0.003(2) -0.006(2) -0.008(2) C4 0.030(3) 0.032(3) 0.026(2) -0.007(2) -0.006(2) -0.010(2) C5 0.023(2) 0.032(3) 0.033(3) -0.006(2) -0.008(2) -0.009(2) C6 0.022(2) 0.029(3) 0.033(3) -0.002(2) -0.003(2) -0.009(2) C7 0.034(3) 0.035(3) 0.038(3) -0.012(2) 0.005(2) -0.009(2) C8 0.047(3) 0.041(3) 0.036(3) -0.014(2) 0.007(2) -0.010(3) C9 0.030(3) 0.082(5) 0.078(5) -0.044(4) -0.002(3) 0.004(3) C10 0.048(3) 0.032(3) 0.030(3) -0.003(2) -0.002(2) -0.018(2) C11 0.060(4) 0.043(3) 0.036(3) 0.004(3) -0.014(3) -0.007(3) C12 0.048(4) 0.067(4) 0.042(3) 0.010(3) 0.007(3) -0.019(3) C13 0.034(3) 0.032(3) 0.039(3) -0.008(2) -0.002(2) -0.012(2) C14 0.052(4) 0.029(3) 0.053(3) -0.002(2) -0.008(3) -0.016(3) C15 0.074(4) 0.041(3) 0.073(4) -0.009(3) -0.033(4) -0.026(3) C16 0.024(2) 0.027(3) 0.034(3) -0.003(2) -0.008(2) -0.007(2) C17 0.019(2) 0.034(3) 0.031(3) -0.003(2) -0.003(2) -0.008(2) C18 0.020(2) 0.031(3) 0.029(2) -0.007(2) -0.003(2) -0.005(2) C19 0.023(2) 0.022(2) 0.030(2) -0.004(2) -0.004(2) -0.0003(19) C20 0.023(2) 0.033(3) 0.026(2) -0.001(2) -0.006(2) -0.005(2) C21 0.024(2) 0.032(3) 0.028(2) -0.005(2) -0.007(2) -0.006(2) C22 0.035(3) 0.035(3) 0.046(3) -0.014(2) 0.002(2) -0.010(2) C23 0.051(4) 0.035(3) 0.062(4) -0.006(3) -0.006(3) -0.018(3) C24 0.064(4) 0.057(4) 0.065(4) -0.012(3) -0.021(3) -0.029(3) C25 0.029(3) 0.033(3) 0.036(3) -0.008(2) -0.001(2) -0.002(2) C26 0.033(3) 0.069(4) 0.070(4) -0.034(4) -0.006(3) 0.007(3) C27 0.043(3) 0.048(3) 0.045(3) -0.023(3) 0.005(3) -0.009(3) C28 0.038(3) 0.039(3) 0.025(2) -0.002(2) -0.003(2) -0.013(2) C29 0.043(3) 0.065(4) 0.038(3) 0.009(3) 0.006(3) -0.013(3) C30 0.050(3) 0.036(3) 0.030(3) 0.000(2) -0.007(2) -0.009(2) C31 0.034(3) 0.026(3) 0.028(3) -0.005(2) 0.001(2) -0.005(2) C32 0.035(3) 0.030(3) 0.025(2) -0.008(2) 0.002(2) -0.008(2) C33 0.038(3) 0.029(3) 0.027(2) -0.004(2) 0.002(2) -0.007(2) C34 0.037(3) 0.025(3) 0.029(3) -0.005(2) 0.004(2) -0.007(2) C35 0.031(3) 0.024(2) 0.033(3) -0.007(2) 0.002(2) -0.004(2) C36 0.028(3) 0.029(3) 0.033(3) -0.007(2) 0.001(2) -0.011(2) C37 0.036(3) 0.048(3) 0.033(3) -0.014(2) 0.003(2) -0.007(2) C38 0.035(3) 0.039(3) 0.031(3) -0.014(2) 0.001(2) -0.012(2) C39 0.029(3) 0.081(5) 0.081(5) -0.026(4) 0.001(3) -0.004(3) C40 0.049(3) 0.030(3) 0.028(3) -0.009(2) 0.002(2) -0.006(2) C41 0.065(4) 0.045(3) 0.051(4) -0.014(3) -0.022(3) -0.012(3) C42 0.047(3) 0.038(3) 0.028(3) -0.008(2) 0.009(2) -0.007(3) C43 0.043(4) 0.090(5) 0.059(4) -0.013(4) 0.021(3) -0.018(4) C44 0.034(3) 0.028(3) 0.029(3) -0.005(2) 0.004(2) -0.005(2) C45 0.039(3) 0.052(4) 0.060(4) -0.016(3) -0.002(3) -0.017(3) O1S 0.116(7) 0.216(10) 0.155(8) 0.015(7) -0.008(6) -0.021(7) O2S 0.105(6) 0.284(12) 0.127(7) -0.029(7) 0.012(5) -0.067(7) C1S 0.39(3) 0.29(2) 0.073(7) 0.011(9) -0.091(11) -0.24(2) C2S 0.073(5) 0.108(7) 0.084(6) -0.033(5) -0.018(5) -0.022(5) C3S 0.043(6) 0.36(3) 0.50(4) -0.31(3) -0.086(13) 0.054(10) C4S 0.201(17) 0.65(4) 0.104(10) -0.169(18) 0.044(11) -0.24(2) C5S 0.242(18) 0.216(15) 0.061(6) 0.027(8) -0.042(8) -0.116(13) C6S 0.33(2) 0.31(2) 0.31(2) 0.199(19) -0.28(2) -0.26(2) C7S 0.059(6) 0.093(7) 0.271(17) 0.023(9) -0.053(8) -0.043(5) C8S 0.095(10) 0.52(4) 0.147(12) -0.099(17) 0.048(9) -0.141(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C6 2.277(4) . ? Mo1 C4 2.278(4) . ? Mo1 C2 2.290(5) . ? Mo1 C1 2.304(5) . ? Mo1 C5 2.305(4) . ? Mo1 C3 2.313(4) . ? Mo2 C21 2.279(4) . ? Mo2 C17 2.286(4) . ? Mo2 C19 2.294(4) . ? Mo2 C16 2.305(4) . ? Mo2 C20 2.308(4) . ? Mo2 C18 2.313(4) . ? O1 C36 1.209(6) . ? O2 C36 1.343(6) . ? O2 C37 1.445(6) . ? O3 C38 1.205(6) . ? O4 C38 1.351(6) . ? O4 C39 1.439(7) . ? O5 C40 1.206(6) . ? O6 C40 1.354(6) . ? O6 C41 1.436(6) . ? O7 C42 1.208(6) . ? O8 C42 1.333(6) . ? O8 C43 1.453(7) . ? O9 C44 1.205(6) . ? O10 C44 1.348(6) . ? O10 C45 1.432(6) . ? C1 C2 1.426(6) . ? C1 C6 1.427(6) . ? C1 C7 1.520(7) . ? C2 C3 1.413(7) . ? C3 C4 1.424(6) . ? C3 C10 1.517(6) . ? C4 C5 1.422(6) . ? C5 C6 1.404(7) . ? C5 C13 1.514(7) . ? C7 C8 1.527(7) . ? C7 C9 1.534(8) . ? C10 C12 1.522(8) . ? C10 C11 1.534(7) . ? C13 C14 1.516(7) . ? C13 C15 1.524(7) . ? C16 C17 1.422(7) . ? C16 C21 1.426(6) . ? C16 C22 1.520(7) . ? C17 C18 1.416(7) . ? C18 C19 1.422(6) . ? C18 C25 1.520(7) . ? C19 C20 1.412(6) . ? C20 C21 1.419(7) . ? C20 C28 1.531(6) . ? C22 C23 1.518(8) . ? C22 C24 1.525(7) . ? C25 C27 1.520(7) . ? C25 C26 1.531(7) . ? C28 C29 1.524(8) . ? C28 C30 1.527(7) . ? C31 C32 1.408(7) . ? C31 C35 1.415(7) . ? C31 C36 1.470(7) . ? C32 C33 1.416(7) . ? C32 C38 1.465(7) . ? C33 C34 1.399(7) . ? C33 C40 1.471(7) . ? C34 C35 1.423(7) . ? C34 C42 1.470(7) . ? C35 C44 1.456(7) . ? O1S C1S 1.408(11) . ? O1S C4S 1.524(13) . ? O2S C5S 1.416(11) . ? O2S C8S 1.476(11) . ? C1S C2S 1.306(12) . ? C2S C3S 1.459(12) . ? C3S C4S 1.358(13) . ? C5S C6S 1.356(12) . ? C6S C7S 1.404(13) . ? C7S C8S 1.288(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Mo1 C6 180.0000(10) 2_566 . ? C6 Mo1 C4 64.16(17) 2_566 2_566 ? C6 Mo1 C4 115.84(17) . 2_566 ? C6 Mo1 C4 115.84(17) 2_566 . ? C6 Mo1 C4 64.16(17) . . ? C4 Mo1 C4 180.0000(10) 2_566 . ? C6 Mo1 C2 64.70(16) 2_566 2_566 ? C6 Mo1 C2 115.30(16) . 2_566 ? C4 Mo1 C2 64.27(17) 2_566 2_566 ? C4 Mo1 C2 115.73(17) . 2_566 ? C6 Mo1 C2 115.30(16) 2_566 . ? C6 Mo1 C2 64.70(16) . . ? C4 Mo1 C2 115.73(17) 2_566 . ? C4 Mo1 C2 64.27(17) . . ? C2 Mo1 C2 180.0000(10) 2_566 . ? C6 Mo1 C1 143.71(16) 2_566 . ? C6 Mo1 C1 36.29(16) . . ? C4 Mo1 C1 103.70(17) 2_566 . ? C4 Mo1 C1 76.30(17) . . ? C2 Mo1 C1 143.82(16) 2_566 . ? C2 Mo1 C1 36.18(16) . . ? C6 Mo1 C1 36.29(16) 2_566 2_566 ? C6 Mo1 C1 143.71(16) . 2_566 ? C4 Mo1 C1 76.30(17) 2_566 2_566 ? C4 Mo1 C1 103.70(17) . 2_566 ? C2 Mo1 C1 36.18(16) 2_566 2_566 ? C2 Mo1 C1 143.82(16) . 2_566 ? C1 Mo1 C1 180.0(2) . 2_566 ? C6 Mo1 C5 35.68(17) 2_566 2_566 ? C6 Mo1 C5 144.32(17) . 2_566 ? C4 Mo1 C5 36.14(16) 2_566 2_566 ? C4 Mo1 C5 143.86(16) . 2_566 ? C2 Mo1 C5 76.53(16) 2_566 2_566 ? C2 Mo1 C5 103.47(16) . 2_566 ? C1 Mo1 C5 114.89(17) . 2_566 ? C1 Mo1 C5 65.11(17) 2_566 2_566 ? C6 Mo1 C5 144.32(17) 2_566 . ? C6 Mo1 C5 35.68(17) . . ? C4 Mo1 C5 143.86(16) 2_566 . ? C4 Mo1 C5 36.14(16) . . ? C2 Mo1 C5 103.47(16) 2_566 . ? C2 Mo1 C5 76.53(16) . . ? C1 Mo1 C5 65.11(17) . . ? C1 Mo1 C5 114.89(17) 2_566 . ? C5 Mo1 C5 180.00(19) 2_566 . ? C6 Mo1 C3 76.39(16) 2_566 2_566 ? C6 Mo1 C3 103.61(16) . 2_566 ? C4 Mo1 C3 36.12(16) 2_566 2_566 ? C4 Mo1 C3 143.88(16) . 2_566 ? C2 Mo1 C3 35.75(16) 2_566 2_566 ? C2 Mo1 C3 144.25(16) . 2_566 ? C1 Mo1 C3 114.99(17) . 2_566 ? C1 Mo1 C3 65.01(17) 2_566 2_566 ? C5 Mo1 C3 65.34(16) 2_566 2_566 ? C5 Mo1 C3 114.66(16) . 2_566 ? C6 Mo1 C3 103.61(16) 2_566 . ? C6 Mo1 C3 76.39(16) . . ? C4 Mo1 C3 143.88(16) 2_566 . ? C4 Mo1 C3 36.12(16) . . ? C2 Mo1 C3 144.25(16) 2_566 . ? C2 Mo1 C3 35.75(16) . . ? C1 Mo1 C3 65.01(17) . . ? C1 Mo1 C3 114.99(17) 2_566 . ? C5 Mo1 C3 114.66(16) 2_566 . ? C5 Mo1 C3 65.34(16) . . ? C3 Mo1 C3 180.00(15) 2_566 . ? C21 Mo2 C21 180.0(2) . 2_665 ? C21 Mo2 C17 115.43(17) . 2_665 ? C21 Mo2 C17 64.57(17) 2_665 2_665 ? C21 Mo2 C17 64.57(17) . . ? C21 Mo2 C17 115.43(17) 2_665 . ? C17 Mo2 C17 180.0(2) 2_665 . ? C21 Mo2 C19 115.66(16) . 2_665 ? C21 Mo2 C19 64.34(16) 2_665 2_665 ? C17 Mo2 C19 64.04(16) 2_665 2_665 ? C17 Mo2 C19 115.96(16) . 2_665 ? C21 Mo2 C19 64.34(16) . . ? C21 Mo2 C19 115.66(16) 2_665 . ? C17 Mo2 C19 115.96(16) 2_665 . ? C17 Mo2 C19 64.04(16) . . ? C19 Mo2 C19 180.0(2) 2_665 . ? C21 Mo2 C16 143.75(16) . 2_665 ? C21 Mo2 C16 36.25(16) 2_665 2_665 ? C17 Mo2 C16 36.08(17) 2_665 2_665 ? C17 Mo2 C16 143.92(17) . 2_665 ? C19 Mo2 C16 76.27(16) 2_665 2_665 ? C19 Mo2 C16 103.73(16) . 2_665 ? C21 Mo2 C16 36.25(16) . . ? C21 Mo2 C16 143.75(16) 2_665 . ? C17 Mo2 C16 143.92(17) 2_665 . ? C17 Mo2 C16 36.08(17) . . ? C19 Mo2 C16 103.73(16) 2_665 . ? C19 Mo2 C16 76.27(16) . . ? C16 Mo2 C16 180.0(3) 2_665 . ? C21 Mo2 C20 36.04(16) . . ? C21 Mo2 C20 143.96(16) 2_665 . ? C17 Mo2 C20 103.98(16) 2_665 . ? C17 Mo2 C20 76.02(16) . . ? C19 Mo2 C20 144.27(16) 2_665 . ? C19 Mo2 C20 35.73(16) . . ? C16 Mo2 C20 114.90(16) 2_665 . ? C16 Mo2 C20 65.10(16) . . ? C21 Mo2 C20 143.96(16) . 2_665 ? C21 Mo2 C20 36.04(16) 2_665 2_665 ? C17 Mo2 C20 76.02(16) 2_665 2_665 ? C17 Mo2 C20 103.98(16) . 2_665 ? C19 Mo2 C20 35.73(16) 2_665 2_665 ? C19 Mo2 C20 144.27(16) . 2_665 ? C16 Mo2 C20 65.10(16) 2_665 2_665 ? C16 Mo2 C20 114.90(16) . 2_665 ? C20 Mo2 C20 180.00(14) . 2_665 ? C21 Mo2 C18 76.62(16) . . ? C21 Mo2 C18 103.38(16) 2_665 . ? C17 Mo2 C18 144.14(16) 2_665 . ? C17 Mo2 C18 35.86(16) . . ? C19 Mo2 C18 144.05(16) 2_665 . ? C19 Mo2 C18 35.95(16) . . ? C16 Mo2 C18 114.82(16) 2_665 . ? C16 Mo2 C18 65.18(16) . . ? C20 Mo2 C18 64.89(16) . . ? C20 Mo2 C18 115.11(16) 2_665 . ? C21 Mo2 C18 103.38(16) . 2_665 ? C21 Mo2 C18 76.62(16) 2_665 2_665 ? C17 Mo2 C18 35.86(16) 2_665 2_665 ? C17 Mo2 C18 144.14(16) . 2_665 ? C19 Mo2 C18 35.95(16) 2_665 2_665 ? C19 Mo2 C18 144.05(16) . 2_665 ? C16 Mo2 C18 65.18(16) 2_665 2_665 ? C16 Mo2 C18 114.82(16) . 2_665 ? C20 Mo2 C18 115.11(16) . 2_665 ? C20 Mo2 C18 64.89(16) 2_665 2_665 ? C18 Mo2 C18 180.0(2) . 2_665 ? C36 O2 C37 115.2(4) . . ? C38 O4 C39 115.8(5) . . ? C40 O6 C41 115.9(4) . . ? C42 O8 C43 116.6(5) . . ? C44 O10 C45 117.1(4) . . ? C2 C1 C6 117.9(4) . . ? C2 C1 C7 122.0(4) . . ? C6 C1 C7 119.9(4) . . ? C2 C1 Mo1 71.4(3) . . ? C6 C1 Mo1 70.8(3) . . ? C7 C1 Mo1 133.3(3) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 Mo1 73.0(3) . . ? C1 C2 Mo1 72.4(3) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 C10 120.7(4) . . ? C4 C3 C10 121.2(4) . . ? C2 C3 Mo1 71.2(3) . . ? C4 C3 Mo1 70.6(3) . . ? C10 C3 Mo1 134.4(3) . . ? C5 C4 C3 122.4(4) . . ? C5 C4 Mo1 72.9(3) . . ? C3 C4 Mo1 73.3(3) . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C13 122.2(4) . . ? C4 C5 C13 119.8(4) . . ? C6 C5 Mo1 71.1(3) . . ? C4 C5 Mo1 70.9(2) . . ? C13 C5 Mo1 133.8(3) . . ? C5 C6 C1 122.3(4) . . ? C5 C6 Mo1 73.2(3) . . ? C1 C6 Mo1 72.9(3) . . ? C1 C7 C8 114.1(4) . . ? C1 C7 C9 108.0(4) . . ? C8 C7 C9 110.2(5) . . ? C3 C10 C12 114.5(4) . . ? C3 C10 C11 108.2(4) . . ? C12 C10 C11 110.7(5) . . ? C5 C13 C14 115.0(4) . . ? C5 C13 C15 109.1(4) . . ? C14 C13 C15 110.4(4) . . ? C17 C16 C21 117.8(4) . . ? C17 C16 C22 122.0(4) . . ? C21 C16 C22 120.1(4) . . ? C17 C16 Mo2 71.2(3) . . ? C21 C16 Mo2 70.9(2) . . ? C22 C16 Mo2 132.4(3) . . ? C18 C17 C16 122.5(4) . . ? C18 C17 Mo2 73.1(3) . . ? C16 C17 Mo2 72.7(3) . . ? C17 C18 C19 117.6(4) . . ? C17 C18 C25 119.8(4) . . ? C19 C18 C25 122.2(4) . . ? C17 C18 Mo2 71.0(3) . . ? C19 C18 Mo2 71.3(3) . . ? C25 C18 Mo2 133.6(3) . . ? C20 C19 C18 122.0(4) . . ? C20 C19 Mo2 72.7(3) . . ? C18 C19 Mo2 72.8(3) . . ? C19 C20 C21 118.6(4) . . ? C19 C20 C28 120.2(4) . . ? C21 C20 C28 121.0(4) . . ? C19 C20 Mo2 71.6(2) . . ? C21 C20 Mo2 70.9(2) . . ? C28 C20 Mo2 133.5(3) . . ? C20 C21 C16 121.4(4) . . ? C20 C21 Mo2 73.1(3) . . ? C16 C21 Mo2 72.9(3) . . ? C23 C22 C16 114.4(4) . . ? C23 C22 C24 109.7(5) . . ? C16 C22 C24 109.3(4) . . ? C18 C25 C27 114.4(4) . . ? C18 C25 C26 108.2(4) . . ? C27 C25 C26 110.8(5) . . ? C29 C28 C30 110.5(4) . . ? C29 C28 C20 114.1(4) . . ? C30 C28 C20 107.8(4) . . ? C32 C31 C35 108.1(4) . . ? C32 C31 C36 126.5(4) . . ? C35 C31 C36 125.4(4) . . ? C31 C32 C33 108.1(4) . . ? C31 C32 C38 125.6(4) . . ? C33 C32 C38 126.2(4) . . ? C34 C33 C32 108.1(4) . . ? C34 C33 C40 127.1(4) . . ? C32 C33 C40 124.8(5) . . ? C33 C34 C35 108.3(4) . . ? C33 C34 C42 125.7(5) . . ? C35 C34 C42 125.5(5) . . ? C31 C35 C34 107.4(4) . . ? C31 C35 C44 126.3(4) . . ? C34 C35 C44 126.3(4) . . ? O1 C36 O2 123.0(4) . . ? O1 C36 C31 124.8(5) . . ? O2 C36 C31 112.2(4) . . ? O3 C38 O4 122.3(5) . . ? O3 C38 C32 126.1(5) . . ? O4 C38 C32 111.6(4) . . ? O5 C40 O6 122.4(5) . . ? O5 C40 C33 126.7(5) . . ? O6 C40 C33 110.9(4) . . ? O7 C42 O8 122.7(5) . . ? O7 C42 C34 124.3(5) . . ? O8 C42 C34 113.0(4) . . ? O9 C44 O10 122.3(5) . . ? O9 C44 C35 126.3(5) . . ? O10 C44 C35 111.3(4) . . ? C1S O1S C4S 104.9(10) . . ? C5S O2S C8S 101.6(10) . . ? C2S C1S O1S 111.8(12) . . ? C1S C2S C3S 103.7(10) . . ? C4S C3S C2S 109.5(10) . . ? C3S C4S O1S 101.1(10) . . ? C6S C5S O2S 104.1(10) . . ? C5S C6S C7S 115.1(9) . . ? C8S C7S C6S 101.6(9) . . ? C7S C8S O2S 114.5(11) . . ? #===END # Attachment 'Momesitylene.cif' data_gp60 _database_code_depnum_ccdc_archive 'CCDC 607084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 O10, C18 H24 Mo' _chemical_formula_sum 'C33 H39 Mo O10' _chemical_formula_weight 691.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 .6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0547(9) _cell_length_b 15.6785(12) _cell_length_c 20.1419(16) _cell_angle_alpha 90.00 _cell_angle_beta 122.744(2) _cell_angle_gamma 90.00 _cell_volume 3201.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3922 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 21.75 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.62 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.7611 _exptl_absorpt_correction_T_max 0.9681 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41121 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7306 _reflns_number_gt 5609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+6.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7306 _refine_ls_number_parameters 404 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.1264(4) 0.3324(2) 0.2131(2) 0.0543(9) Uani 1 1 d . . . O2 O -0.0945(4) 0.2551(3) 0.3142(2) 0.0600(10) Uani 1 1 d . . . O3A O 0.2337(7) 0.1180(4) 0.4429(3) 0.0392(15) Uiso 0.50 1 d PD A 1 C23A C 0.2835(12) 0.1125(8) 0.5265(5) 0.059(3) Uiso 0.50 1 d PD A 1 H23A H 0.2425 0.1570 0.5404 0.088 Uiso 0.50 1 calc PR A 1 H23B H 0.3794 0.1203 0.5573 0.088 Uiso 0.50 1 calc PR A 1 H23C H 0.2622 0.0563 0.5381 0.088 Uiso 0.50 1 calc PR A 1 O3B O 0.1748(7) 0.1289(4) 0.4393(4) 0.0468(17) Uiso 0.50 1 d PD A 2 C23B C 0.2181(12) 0.1303(8) 0.5215(5) 0.058(3) Uiso 0.50 1 d PD A 2 H23D H 0.3095 0.1505 0.5532 0.087 Uiso 0.50 1 calc PR A 2 H23E H 0.2127 0.0727 0.5383 0.087 Uiso 0.50 1 calc PR A 2 H23F H 0.1614 0.1688 0.5288 0.087 Uiso 0.50 1 calc PR A 2 O4 O 0.1984(4) 0.2638(3) 0.4449(2) 0.0638(11) Uani 1 1 d . A . O5A O 0.4117(6) 0.1524(4) 0.4284(3) 0.0425(17) Uiso 0.50 1 d PD A 1 C26A C 0.5421(8) 0.1224(7) 0.4890(5) 0.042(2) Uiso 0.50 1 d PD A 1 H26A H 0.5734 0.0815 0.4660 0.063 Uiso 0.50 1 calc PR A 1 H26B H 0.5379 0.0945 0.5312 0.063 Uiso 0.50 1 calc PR A 1 H26C H 0.6029 0.1709 0.5109 0.063 Uiso 0.50 1 calc PR A 1 O5B O 0.4450(6) 0.1556(4) 0.4143(3) 0.0394(16) Uiso 0.50 1 d PD A 2 C26B C 0.5660(9) 0.1121(7) 0.4699(6) 0.050(3) Uiso 0.50 1 d PD A 2 H26D H 0.5482 0.0678 0.4973 0.074 Uiso 0.50 1 calc PR A 2 H26E H 0.6295 0.1531 0.5085 0.074 Uiso 0.50 1 calc PR A 2 H26F H 0.6026 0.0857 0.4416 0.074 Uiso 0.50 1 calc PR A 2 O6 O 0.3941(4) 0.0501(3) 0.3382(2) 0.0679(12) Uani 1 1 d . . . O7 O 0.3081(3) 0.1354(3) 0.17802(19) 0.0645(12) Uani 1 1 d . A . O8A O 0.0957(5) 0.1005(3) 0.0945(3) 0.0260(11) Uiso 0.50 1 d PD A 1 C29A C 0.1214(9) 0.0824(6) 0.0332(5) 0.038(2) Uiso 0.50 1 d PD A 1 H29A H 0.1627 0.1322 0.0258 0.057 Uiso 0.50 1 calc PR A 1 H29B H 0.0381 0.0696 -0.0163 0.057 Uiso 0.50 1 calc PR A 1 H29C H 0.1807 0.0332 0.0489 0.057 Uiso 0.50 1 calc PR A 1 O8B O 0.1309(7) 0.0611(4) 0.1316(4) 0.0587(19) Uiso 0.50 1 d PD A 2 C29B C 0.1681(17) 0.0255(10) 0.0799(9) 0.100(5) Uiso 0.50 1 d PD A 2 H29D H 0.1665 0.0705 0.0456 0.149 Uiso 0.50 1 calc PR A 2 H29E H 0.1057 -0.0196 0.0474 0.149 Uiso 0.50 1 calc PR A 2 H29F H 0.2571 0.0015 0.1117 0.149 Uiso 0.50 1 calc PR A 2 O9 O -0.1758(3) 0.2325(2) 0.07894(18) 0.0414(8) Uani 1 1 d . . . O10A O -0.0027(5) 0.2675(4) 0.0733(3) 0.0263(13) Uiso 0.50 1 d PD A 1 C32A C -0.0906(9) 0.2837(7) -0.0099(4) 0.038(2) Uiso 0.50 1 d PD A 1 H32A H -0.1488 0.2344 -0.0351 0.058 Uiso 0.50 1 calc PR A 1 H32B H -0.0390 0.2932 -0.0337 0.058 Uiso 0.50 1 calc PR A 1 H32C H -0.1438 0.3344 -0.0176 0.058 Uiso 0.50 1 calc PR A 1 O10B O 0.0060(6) 0.2307(4) 0.0710(3) 0.0335(14) Uiso 0.50 1 d PD A 2 C32B C -0.0792(10) 0.2403(8) -0.0133(5) 0.050(3) Uiso 0.50 1 d PD A 2 H32D H -0.1384 0.1910 -0.0354 0.075 Uiso 0.50 1 calc PR A 2 H32E H -0.0258 0.2439 -0.0364 0.075 Uiso 0.50 1 calc PR A 2 H32F H -0.1315 0.2925 -0.0254 0.075 Uiso 0.50 1 calc PR A 2 C19 C -0.0678(5) 0.2704(3) 0.2658(3) 0.0396(11) Uani 1 1 d . . . C20 C 0.0351(4) 0.2263(3) 0.2603(2) 0.0319(9) Uani 1 1 d . A . C21 C 0.1503(4) 0.1939(3) 0.3266(2) 0.0381(11) Uani 1 1 d . A . C22 C 0.1864(5) 0.2001(3) 0.4090(3) 0.0538(15) Uani 1 1 d D . . C24 C 0.2264(4) 0.1549(3) 0.3016(2) 0.0372(10) Uani 1 1 d . . . C25 C 0.3547(5) 0.1123(3) 0.3528(3) 0.0463(13) Uani 1 1 d D A . C27 C 0.1586(4) 0.1629(3) 0.2192(2) 0.0330(9) Uani 1 1 d . A . C28 C 0.2028(4) 0.1291(3) 0.1689(3) 0.0398(11) Uani 1 1 d D . . C30 C 0.0412(4) 0.2078(3) 0.1932(2) 0.0288(9) Uani 1 1 d . . . C31 C -0.0575(4) 0.2301(3) 0.1106(2) 0.0319(9) Uani 1 1 d D A . C33 C -0.2247(6) 0.3819(4) 0.2161(4) 0.0683(17) Uani 1 1 d . . . H33A H -0.2977 0.3447 0.2057 0.102 Uiso 1 1 calc R . . H33B H -0.2579 0.4271 0.1762 0.102 Uiso 1 1 calc R . . H33C H -0.1850 0.4076 0.2686 0.102 Uiso 1 1 calc R . . Mo1 Mo 0.32256(3) 0.49681(2) 0.289035(18) 0.02224(10) Uani 1 1 d . . . C1 C 0.3561(4) 0.4162(3) 0.2078(2) 0.0330(9) Uani 1 1 d . . . C2 C 0.2253(4) 0.4050(3) 0.1867(2) 0.0351(10) Uani 1 1 d . . . H2 H 0.1946 0.3489 0.1860 0.042 Uiso 1 1 calc R . . C3 C 0.1371(4) 0.4748(3) 0.1663(2) 0.0339(10) Uani 1 1 d . . . C4 C 0.1856(4) 0.5585(2) 0.1693(2) 0.0282(8) Uani 1 1 d . . . H4 H 0.1290 0.6061 0.1574 0.034 Uiso 1 1 calc R . . C5 C 0.3156(4) 0.5720(2) 0.1897(2) 0.0277(8) Uani 1 1 d . . . C6 C 0.4006(4) 0.5003(3) 0.2091(2) 0.0317(9) Uani 1 1 d . . . H6 H 0.4888 0.5091 0.2233 0.038 Uiso 1 1 calc R . . C7 C 0.3657(4) 0.6605(3) 0.1915(3) 0.0352(10) Uani 1 1 d . . . H7A H 0.4587 0.6646 0.2345 0.053 Uiso 1 1 calc R . . H7B H 0.3141 0.7021 0.2001 0.053 Uiso 1 1 calc R . . H7C H 0.3569 0.6724 0.1411 0.053 Uiso 1 1 calc R . . C8 C -0.0024(5) 0.4614(4) 0.1419(3) 0.0548(14) Uani 1 1 d . . . H8A H -0.0332 0.5113 0.1567 0.082 Uiso 1 1 calc R . . H8B H -0.0081 0.4106 0.1683 0.082 Uiso 1 1 calc R . . H8C H -0.0576 0.4534 0.0845 0.082 Uiso 1 1 calc R . . C9 C 0.4462(6) 0.3410(3) 0.2278(3) 0.0531(14) Uani 1 1 d . . . H9A H 0.4410 0.3211 0.1801 0.080 Uiso 1 1 calc R . . H9B H 0.4192 0.2949 0.2491 0.080 Uiso 1 1 calc R . . H9C H 0.5370 0.3579 0.2674 0.080 Uiso 1 1 calc R . . C10 C 0.2486(4) 0.4942(3) 0.3726(2) 0.0305(8) Uani 1 1 d . . . C11 C 0.3308(4) 0.4222(3) 0.3883(2) 0.0308(9) Uani 1 1 d . . . H11 H 0.2974 0.3667 0.3862 0.037 Uiso 1 1 calc R . . C12 C 0.4611(4) 0.4313(3) 0.4068(2) 0.0316(9) Uani 1 1 d . . . C13 C 0.5088(4) 0.5146(3) 0.4096(2) 0.0314(9) Uani 1 1 d . . . H13 H 0.5964 0.5214 0.4220 0.038 Uiso 1 1 calc R . . C14 C 0.4307(4) 0.5879(2) 0.3945(2) 0.0291(9) Uani 1 1 d . . . C15 C 0.2994(4) 0.5767(3) 0.3750(2) 0.0282(8) Uani 1 1 d . . . H15 H 0.2446 0.6252 0.3634 0.034 Uiso 1 1 calc R . . C16 C 0.4857(5) 0.6758(3) 0.3988(3) 0.0389(10) Uani 1 1 d . . . H16A H 0.5323 0.6964 0.4534 0.058 Uiso 1 1 calc R . . H16B H 0.4133 0.7149 0.3647 0.058 Uiso 1 1 calc R . . H16C H 0.5471 0.6730 0.3812 0.058 Uiso 1 1 calc R . . C17 C 0.5481(5) 0.3545(3) 0.4238(3) 0.0432(11) Uani 1 1 d . . . H17A H 0.6035 0.3453 0.4809 0.065 Uiso 1 1 calc R . . H17B H 0.6043 0.3643 0.4031 0.065 Uiso 1 1 calc R . . H17C H 0.4929 0.3041 0.3984 0.065 Uiso 1 1 calc R . . C18 C 0.1100(5) 0.4845(3) 0.3534(3) 0.0453(12) Uani 1 1 d . . . H18A H 0.1074 0.4998 0.3998 0.068 Uiso 1 1 calc R . . H18B H 0.0813 0.4252 0.3387 0.068 Uiso 1 1 calc R . . H18C H 0.0509 0.5223 0.3094 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.067(2) 0.053(2) 0.058(2) -0.0002(18) 0.043(2) 0.0042(18) O2 0.067(3) 0.074(3) 0.064(2) -0.009(2) 0.052(2) -0.020(2) O4 0.077(3) 0.082(3) 0.0337(19) -0.0117(19) 0.031(2) -0.027(2) O6 0.048(2) 0.111(4) 0.044(2) 0.013(2) 0.0243(19) 0.018(2) O7 0.0315(18) 0.133(4) 0.0317(18) -0.006(2) 0.0191(15) -0.024(2) O9 0.0333(17) 0.0508(19) 0.0319(16) 0.0027(14) 0.0124(14) -0.0105(14) C19 0.042(3) 0.043(3) 0.032(2) -0.010(2) 0.019(2) -0.022(2) C20 0.035(2) 0.036(2) 0.025(2) -0.0040(17) 0.0158(18) -0.0141(17) C21 0.042(3) 0.042(2) 0.024(2) -0.0019(18) 0.0134(19) -0.022(2) C22 0.062(3) 0.060(3) 0.027(2) -0.006(2) 0.016(2) -0.039(3) C24 0.033(2) 0.040(2) 0.030(2) 0.0062(18) 0.0117(19) -0.0154(19) C25 0.040(3) 0.052(3) 0.038(3) 0.014(2) 0.015(2) -0.020(2) C27 0.027(2) 0.036(2) 0.032(2) 0.0024(17) 0.0134(18) -0.0136(17) C28 0.032(2) 0.046(3) 0.039(2) -0.002(2) 0.018(2) -0.013(2) C30 0.029(2) 0.033(2) 0.0225(19) -0.0033(16) 0.0130(17) -0.0150(17) C31 0.030(2) 0.038(2) 0.023(2) -0.0031(17) 0.0113(18) -0.0135(18) C33 0.058(4) 0.070(4) 0.078(4) -0.017(3) 0.038(3) 0.001(3) Mo1 0.02474(17) 0.01997(16) 0.02058(16) 0.00101(13) 0.01132(13) 0.00139(13) C1 0.044(3) 0.028(2) 0.0211(19) -0.0035(16) 0.0136(18) 0.0074(18) C2 0.043(3) 0.024(2) 0.025(2) 0.0006(16) 0.0095(19) -0.0048(18) C3 0.033(2) 0.031(2) 0.028(2) 0.0052(17) 0.0101(18) -0.0062(17) C4 0.028(2) 0.0267(19) 0.0242(19) 0.0023(15) 0.0108(17) -0.0012(16) C5 0.031(2) 0.027(2) 0.0228(19) 0.0015(15) 0.0132(17) -0.0024(16) C6 0.036(2) 0.039(2) 0.0249(19) 0.0019(18) 0.0197(17) 0.0042(19) C7 0.031(2) 0.032(2) 0.034(2) 0.0074(18) 0.0119(19) -0.0032(18) C8 0.033(3) 0.059(3) 0.057(3) 0.014(3) 0.014(2) -0.014(2) C9 0.077(4) 0.042(3) 0.035(3) 0.001(2) 0.028(3) 0.027(3) C10 0.033(2) 0.037(2) 0.0259(19) 0.0017(17) 0.0184(17) 0.0010(18) C11 0.039(2) 0.027(2) 0.027(2) 0.0031(16) 0.0179(19) -0.0009(17) C12 0.031(2) 0.036(2) 0.0201(19) 0.0027(16) 0.0093(17) 0.0043(18) C13 0.0252(19) 0.039(2) 0.0240(19) -0.0041(17) 0.0092(16) 0.0008(17) C14 0.032(2) 0.028(2) 0.0236(19) -0.0038(16) 0.0127(17) -0.0036(17) C15 0.033(2) 0.030(2) 0.0233(19) -0.0007(16) 0.0165(17) 0.0051(17) C16 0.046(3) 0.032(2) 0.038(2) -0.0093(19) 0.022(2) -0.011(2) C17 0.046(3) 0.042(3) 0.028(2) 0.0053(19) 0.012(2) 0.018(2) C18 0.042(3) 0.047(3) 0.060(3) 0.000(2) 0.036(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C19 1.327(6) . ? O1 C33 1.445(6) . ? O2 C19 1.205(5) . ? O3A C22 1.423(6) . ? O3A C23A 1.452(7) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? O3B C22 1.315(6) . ? O3B C23B 1.442(7) . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? O4 C22 1.196(6) . ? O5A C25 1.434(6) . ? O5A C26A 1.452(7) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? O5B C25 1.312(6) . ? O5B C26B 1.442(7) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? O6 C25 1.189(6) . ? O7 C28 1.185(5) . ? O8A C28 1.422(5) . ? O8A C29A 1.454(7) . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? O8B C28 1.323(6) . ? O8B C29B 1.449(8) . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? O9 C31 1.207(5) . ? O10A C31 1.371(5) . ? O10A C32A 1.441(7) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? O10B C31 1.372(6) . ? O10B C32B 1.441(7) . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C19 C20 1.475(7) . ? C20 C21 1.401(6) . ? C20 C30 1.423(5) . ? C21 C24 1.404(7) . ? C21 C22 1.473(6) . ? C24 C27 1.405(6) . ? C24 C25 1.475(7) . ? C27 C30 1.404(6) . ? C27 C28 1.473(6) . ? C30 C31 1.472(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Mo1 C2 2.255(4) . ? Mo1 C6 2.262(4) . ? Mo1 C13 2.262(4) . ? Mo1 C1 2.270(4) . ? Mo1 C11 2.271(4) . ? Mo1 C4 2.273(4) . ? Mo1 C15 2.274(4) . ? Mo1 C12 2.276(4) . ? Mo1 C5 2.284(4) . ? Mo1 C3 2.291(4) . ? Mo1 C10 2.293(4) . ? Mo1 C14 2.293(4) . ? C1 C2 1.405(6) . ? C1 C6 1.419(6) . ? C1 C9 1.502(6) . ? C2 C3 1.422(6) . ? C2 H2 0.9500 . ? C3 C4 1.424(5) . ? C3 C8 1.490(6) . ? C4 C5 1.405(6) . ? C4 H4 0.9500 . ? C5 C6 1.425(5) . ? C5 C7 1.506(5) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.420(6) . ? C10 C11 1.421(6) . ? C10 C18 1.505(6) . ? C11 C12 1.411(6) . ? C11 H11 0.9500 . ? C12 C13 1.416(6) . ? C12 C17 1.510(6) . ? C13 C14 1.411(6) . ? C13 H13 0.9500 . ? C14 C15 1.421(6) . ? C14 C16 1.510(5) . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 O1 C33 117.0(4) . . ? C22 O3A C23A 114.7(7) . . ? C22 O3B C23B 117.2(7) . . ? O3B C23B H23D 109.5 . . ? O3B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? O3B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C25 O5A C26A 115.4(7) . . ? C25 O5B C26B 117.5(7) . . ? O5B C26B H26D 109.5 . . ? O5B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? O5B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28 O8A C29A 117.9(5) . . ? C28 O8B C29B 110.9(9) . . ? O8B C29B H29D 109.5 . . ? O8B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? O8B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C31 O10A C32A 116.3(6) . . ? C31 O10B C32B 114.8(6) . . ? O10B C32B H32D 109.5 . . ? O10B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? O10B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? O2 C19 O1 122.3(5) . . ? O2 C19 C20 124.7(5) . . ? O1 C19 C20 112.9(4) . . ? C21 C20 C30 107.3(4) . . ? C21 C20 C19 122.6(4) . . ? C30 C20 C19 130.1(4) . . ? C20 C21 C24 108.6(4) . . ? C20 C21 C22 125.9(5) . . ? C24 C21 C22 125.5(4) . . ? O4 C22 O3B 115.9(5) . . ? O4 C22 O3A 125.4(5) . . ? O3B C22 O3A 29.1(4) . . ? O4 C22 C21 127.0(4) . . ? O3B C22 C21 115.2(5) . . ? O3A C22 C21 106.2(5) . . ? C21 C24 C27 108.0(4) . . ? C21 C24 C25 126.0(4) . . ? C27 C24 C25 125.9(4) . . ? O6 C25 O5B 114.8(6) . . ? O6 C25 O5A 126.6(5) . . ? O5B C25 O5A 25.0(4) . . ? O6 C25 C24 127.3(4) . . ? O5B C25 C24 116.5(5) . . ? O5A C25 C24 105.2(5) . . ? C30 C27 C24 108.0(4) . . ? C30 C27 C28 126.2(4) . . ? C24 C27 C28 125.7(4) . . ? O7 C28 O8B 118.2(6) . . ? O7 C28 O8A 118.3(4) . . ? O8B C28 O8A 37.2(4) . . ? O7 C28 C27 128.3(4) . . ? O8B C28 C27 108.2(5) . . ? O8A C28 C27 112.3(4) . . ? C27 C30 C20 108.0(4) . . ? C27 C30 C31 125.2(4) . . ? C20 C30 C31 126.8(4) . . ? O9 C31 O10A 118.6(4) . . ? O9 C31 O10B 124.3(4) . . ? O10A C31 O10B 24.9(3) . . ? O9 C31 C30 127.3(4) . . ? O10A C31 C30 112.7(4) . . ? O10B C31 C30 107.1(4) . . ? O1 C33 H33A 109.5 . . ? O1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C2 Mo1 C6 64.90(16) . . ? C2 Mo1 C13 141.61(15) . . ? C6 Mo1 C13 101.98(15) . . ? C2 Mo1 C1 36.17(16) . . ? C6 Mo1 C1 36.49(15) . . ? C13 Mo1 C1 112.46(15) . . ? C2 Mo1 C11 103.25(15) . . ? C6 Mo1 C11 143.28(15) . . ? C13 Mo1 C11 64.75(15) . . ? C1 Mo1 C11 114.03(15) . . ? C2 Mo1 C4 65.28(14) . . ? C6 Mo1 C4 65.04(15) . . ? C13 Mo1 C4 144.65(15) . . ? C1 Mo1 C4 77.46(15) . . ? C11 Mo1 C4 144.44(15) . . ? C2 Mo1 C15 146.18(16) . . ? C6 Mo1 C15 142.98(15) . . ? C13 Mo1 C15 64.78(14) . . ? C1 Mo1 C15 177.24(15) . . ? C11 Mo1 C15 65.06(14) . . ? C4 Mo1 C15 104.81(14) . . ? C2 Mo1 C12 112.97(15) . . ? C6 Mo1 C12 113.54(15) . . ? C13 Mo1 C12 36.35(14) . . ? C1 Mo1 C12 100.57(15) . . ? C11 Mo1 C12 36.15(15) . . ? C4 Mo1 C12 178.02(15) . . ? C15 Mo1 C12 77.16(14) . . ? C2 Mo1 C5 76.95(14) . . ? C6 Mo1 C5 36.53(14) . . ? C13 Mo1 C5 114.92(15) . . ? C1 Mo1 C5 65.95(15) . . ? C11 Mo1 C5 179.65(15) . . ? C4 Mo1 C5 35.91(14) . . ? C15 Mo1 C5 114.94(14) . . ? C12 Mo1 C5 143.50(15) . . ? C2 Mo1 C3 36.46(15) . . ? C6 Mo1 C3 76.94(16) . . ? C13 Mo1 C3 178.04(15) . . ? C1 Mo1 C3 65.69(16) . . ? C11 Mo1 C3 115.15(15) . . ? C4 Mo1 C3 36.36(14) . . ? C15 Mo1 C3 117.07(16) . . ? C12 Mo1 C3 142.56(15) . . ? C5 Mo1 C3 65.18(14) . . ? C2 Mo1 C10 116.33(16) . . ? C6 Mo1 C10 178.58(15) . . ? C13 Mo1 C10 76.61(15) . . ? C1 Mo1 C10 144.19(15) . . ? C11 Mo1 C10 36.28(14) . . ? C4 Mo1 C10 116.01(15) . . ? C15 Mo1 C10 36.24(14) . . ? C12 Mo1 C10 65.44(15) . . ? C5 Mo1 C10 143.89(15) . . ? C3 Mo1 C10 104.47(15) . . ? C2 Mo1 C14 177.39(16) . . ? C6 Mo1 C14 113.42(15) . . ? C13 Mo1 C14 36.08(14) . . ? C1 Mo1 C14 141.36(16) . . ? C11 Mo1 C14 76.89(14) . . ? C4 Mo1 C14 116.12(14) . . ? C15 Mo1 C14 36.24(14) . . ? C12 Mo1 C14 65.59(15) . . ? C5 Mo1 C14 102.90(14) . . ? C3 Mo1 C14 145.85(15) . . ? C10 Mo1 C14 65.33(15) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 C9 120.9(4) . . ? C6 C1 C9 120.9(4) . . ? C2 C1 Mo1 71.3(2) . . ? C6 C1 Mo1 71.4(2) . . ? C9 C1 Mo1 128.9(3) . . ? C1 C2 C3 122.1(4) . . ? C1 C2 Mo1 72.5(2) . . ? C3 C2 Mo1 73.2(2) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? Mo1 C2 H2 127.6 . . ? C2 C3 C4 118.2(4) . . ? C2 C3 C8 121.3(4) . . ? C4 C3 C8 120.5(4) . . ? C2 C3 Mo1 70.4(2) . . ? C4 C3 Mo1 71.1(2) . . ? C8 C3 Mo1 130.2(3) . . ? C5 C4 C3 121.2(4) . . ? C5 C4 Mo1 72.5(2) . . ? C3 C4 Mo1 72.5(2) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? Mo1 C4 H4 127.8 . . ? C4 C5 C6 119.0(4) . . ? C4 C5 C7 121.0(4) . . ? C6 C5 C7 120.1(4) . . ? C4 C5 Mo1 71.6(2) . . ? C6 C5 Mo1 70.9(2) . . ? C7 C5 Mo1 129.0(3) . . ? C1 C6 C5 121.3(4) . . ? C1 C6 Mo1 72.1(2) . . ? C5 C6 Mo1 72.6(2) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? Mo1 C6 H6 128.2 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.6(4) . . ? C15 C10 C18 119.9(4) . . ? C11 C10 C18 121.4(4) . . ? C15 C10 Mo1 71.2(2) . . ? C11 C10 Mo1 71.0(2) . . ? C18 C10 Mo1 129.2(3) . . ? C12 C11 C10 121.4(4) . . ? C12 C11 Mo1 72.1(2) . . ? C10 C11 Mo1 72.7(2) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? Mo1 C11 H11 128.1 . . ? C11 C12 C13 118.3(4) . . ? C11 C12 C17 121.1(4) . . ? C13 C12 C17 120.6(4) . . ? C11 C12 Mo1 71.7(2) . . ? C13 C12 Mo1 71.3(2) . . ? C17 C12 Mo1 128.6(3) . . ? C14 C13 C12 122.2(4) . . ? C14 C13 Mo1 73.2(2) . . ? C12 C13 Mo1 72.4(2) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? Mo1 C13 H13 127.8 . . ? C13 C14 C15 118.2(4) . . ? C13 C14 C16 120.6(4) . . ? C15 C14 C16 121.2(4) . . ? C13 C14 Mo1 70.8(2) . . ? C15 C14 Mo1 71.1(2) . . ? C16 C14 Mo1 129.3(3) . . ? C10 C15 C14 121.2(4) . . ? C10 C15 Mo1 72.6(2) . . ? C14 C15 Mo1 72.6(2) . . ? C10 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? Mo1 C15 H15 127.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C33 O1 C19 O2 0.3(7) . . . . ? C33 O1 C19 C20 -177.3(4) . . . . ? O2 C19 C20 C21 -31.6(7) . . . . ? O1 C19 C20 C21 145.9(4) . . . . ? O2 C19 C20 C30 148.3(5) . . . . ? O1 C19 C20 C30 -34.2(6) . . . . ? C30 C20 C21 C24 -0.8(5) . . . . ? C19 C20 C21 C24 179.2(4) . . . . ? C30 C20 C21 C22 178.8(4) . . . . ? C19 C20 C21 C22 -1.2(6) . . . . ? C23B O3B C22 O4 -18.9(11) . . . . ? C23B O3B C22 O3A 98.0(12) . . . . ? C23B O3B C22 C21 175.7(8) . . . . ? C23A O3A C22 O4 8.8(11) . . . . ? C23A O3A C22 O3B -71.1(10) . . . . ? C23A O3A C22 C21 175.9(7) . . . . ? C20 C21 C22 O4 -57.6(8) . . . . ? C24 C21 C22 O4 121.9(6) . . . . ? C20 C21 C22 O3B 105.9(7) . . . . ? C24 C21 C22 O3B -74.6(7) . . . . ? C20 C21 C22 O3A 135.5(5) . . . . ? C24 C21 C22 O3A -44.9(6) . . . . ? C20 C21 C24 C27 0.1(5) . . . . ? C22 C21 C24 C27 -179.5(4) . . . . ? C20 C21 C24 C25 -179.5(4) . . . . ? C22 C21 C24 C25 0.8(7) . . . . ? C26B O5B C25 O6 -18.8(10) . . . . ? C26B O5B C25 O5A 105.5(13) . . . . ? C26B O5B C25 C24 173.5(7) . . . . ? C26A O5A C25 O6 11.6(10) . . . . ? C26A O5A C25 O5B -57.5(10) . . . . ? C26A O5A C25 C24 -178.3(6) . . . . ? C21 C24 C25 O6 143.3(5) . . . . ? C27 C24 C25 O6 -36.2(7) . . . . ? C21 C24 C25 O5B -50.7(7) . . . . ? C27 C24 C25 O5B 129.8(6) . . . . ? C21 C24 C25 O5A -26.7(6) . . . . ? C27 C24 C25 O5A 153.7(5) . . . . ? C21 C24 C27 C30 0.7(5) . . . . ? C25 C24 C27 C30 -179.7(4) . . . . ? C21 C24 C27 C28 -178.7(4) . . . . ? C25 C24 C27 C28 0.9(7) . . . . ? C29B O8B C28 O7 -24.7(11) . . . . ? C29B O8B C28 O8A 75.9(10) . . . . ? C29B O8B C28 C27 179.0(9) . . . . ? C29A O8A C28 O7 -1.3(8) . . . . ? C29A O8A C28 O8B -101.6(9) . . . . ? C29A O8A C28 C27 167.4(5) . . . . ? C30 C27 C28 O7 132.8(5) . . . . ? C24 C27 C28 O7 -48.0(7) . . . . ? C30 C27 C28 O8B -74.1(6) . . . . ? C24 C27 C28 O8B 105.1(6) . . . . ? C30 C27 C28 O8A -34.5(6) . . . . ? C24 C27 C28 O8A 144.7(4) . . . . ? C24 C27 C30 C20 -1.1(4) . . . . ? C28 C27 C30 C20 178.2(4) . . . . ? C24 C27 C30 C31 179.6(4) . . . . ? C28 C27 C30 C31 -1.1(6) . . . . ? C21 C20 C30 C27 1.2(4) . . . . ? C19 C20 C30 C27 -178.8(4) . . . . ? C21 C20 C30 C31 -179.5(4) . . . . ? C19 C20 C30 C31 0.5(7) . . . . ? C32A O10A C31 O9 -18.2(8) . . . . ? C32A O10A C31 O10B 92.3(10) . . . . ? C32A O10A C31 C30 174.0(6) . . . . ? C32B O10B C31 O9 4.0(10) . . . . ? C32B O10B C31 O10A -80.6(10) . . . . ? C32B O10B C31 C30 172.1(7) . . . . ? C27 C30 C31 O9 144.3(5) . . . . ? C20 C30 C31 O9 -34.9(7) . . . . ? C27 C30 C31 O10A -49.3(6) . . . . ? C20 C30 C31 O10A 131.5(5) . . . . ? C27 C30 C31 O10B -23.4(6) . . . . ? C20 C30 C31 O10B 157.4(5) . . . . ? C6 Mo1 C1 C2 -129.8(4) . . . . ? C13 Mo1 C1 C2 150.6(2) . . . . ? C11 Mo1 C1 C2 79.4(3) . . . . ? C4 Mo1 C1 C2 -65.1(2) . . . . ? C15 Mo1 C1 C2 149(3) . . . . ? C12 Mo1 C1 C2 114.7(2) . . . . ? C5 Mo1 C1 C2 -101.0(3) . . . . ? C3 Mo1 C1 C2 -28.6(2) . . . . ? C10 Mo1 C1 C2 52.3(4) . . . . ? C14 Mo1 C1 C2 178.6(2) . . . . ? C2 Mo1 C1 C6 129.8(4) . . . . ? C13 Mo1 C1 C6 -79.5(3) . . . . ? C11 Mo1 C1 C6 -150.8(2) . . . . ? C4 Mo1 C1 C6 64.8(2) . . . . ? C15 Mo1 C1 C6 -81(3) . . . . ? C12 Mo1 C1 C6 -115.5(2) . . . . ? C5 Mo1 C1 C6 28.8(2) . . . . ? C3 Mo1 C1 C6 101.2(3) . . . . ? C10 Mo1 C1 C6 -177.9(2) . . . . ? C14 Mo1 C1 C6 -51.6(3) . . . . ? C2 Mo1 C1 C9 -115.0(5) . . . . ? C6 Mo1 C1 C9 115.2(5) . . . . ? C13 Mo1 C1 C9 35.6(5) . . . . ? C11 Mo1 C1 C9 -35.7(5) . . . . ? C4 Mo1 C1 C9 179.9(5) . . . . ? C15 Mo1 C1 C9 34(3) . . . . ? C12 Mo1 C1 C9 -0.4(5) . . . . ? C5 Mo1 C1 C9 143.9(5) . . . . ? C3 Mo1 C1 C9 -143.7(5) . . . . ? C10 Mo1 C1 C9 -62.7(5) . . . . ? C14 Mo1 C1 C9 63.5(5) . . . . ? C6 C1 C2 C3 0.5(6) . . . . ? C9 C1 C2 C3 -179.0(4) . . . . ? Mo1 C1 C2 C3 56.2(4) . . . . ? C6 C1 C2 Mo1 -55.7(3) . . . . ? C9 C1 C2 Mo1 124.8(4) . . . . ? C6 Mo1 C2 C1 30.3(2) . . . . ? C13 Mo1 C2 C1 -46.9(4) . . . . ? C11 Mo1 C2 C1 -112.8(2) . . . . ? C4 Mo1 C2 C1 103.0(3) . . . . ? C15 Mo1 C2 C1 -177.5(2) . . . . ? C12 Mo1 C2 C1 -76.0(3) . . . . ? C5 Mo1 C2 C1 66.9(2) . . . . ? C3 Mo1 C2 C1 132.7(4) . . . . ? C10 Mo1 C2 C1 -148.9(2) . . . . ? C14 Mo1 C2 C1 -20(3) . . . . ? C6 Mo1 C2 C3 -102.4(3) . . . . ? C13 Mo1 C2 C3 -179.5(2) . . . . ? C1 Mo1 C2 C3 -132.7(4) . . . . ? C11 Mo1 C2 C3 114.6(3) . . . . ? C4 Mo1 C2 C3 -29.7(2) . . . . ? C15 Mo1 C2 C3 49.9(4) . . . . ? C12 Mo1 C2 C3 151.3(2) . . . . ? C5 Mo1 C2 C3 -65.7(2) . . . . ? C10 Mo1 C2 C3 78.4(3) . . . . ? C14 Mo1 C2 C3 -153(3) . . . . ? C1 C2 C3 C4 -1.4(6) . . . . ? Mo1 C2 C3 C4 54.5(3) . . . . ? C1 C2 C3 C8 178.3(4) . . . . ? Mo1 C2 C3 C8 -125.8(4) . . . . ? C1 C2 C3 Mo1 -55.9(4) . . . . ? C6 Mo1 C3 C2 65.2(3) . . . . ? C13 Mo1 C3 C2 9(5) . . . . ? C1 Mo1 C3 C2 28.4(2) . . . . ? C11 Mo1 C3 C2 -77.9(3) . . . . ? C4 Mo1 C3 C2 130.7(4) . . . . ? C15 Mo1 C3 C2 -151.5(2) . . . . ? C12 Mo1 C3 C2 -46.6(4) . . . . ? C5 Mo1 C3 C2 102.0(3) . . . . ? C10 Mo1 C3 C2 -114.9(3) . . . . ? C14 Mo1 C3 C2 177.9(3) . . . . ? C2 Mo1 C3 C4 -130.7(4) . . . . ? C6 Mo1 C3 C4 -65.4(3) . . . . ? C13 Mo1 C3 C4 -122(4) . . . . ? C1 Mo1 C3 C4 -102.2(3) . . . . ? C11 Mo1 C3 C4 151.4(2) . . . . ? C15 Mo1 C3 C4 77.9(3) . . . . ? C12 Mo1 C3 C4 -177.2(2) . . . . ? C5 Mo1 C3 C4 -28.7(2) . . . . ? C10 Mo1 C3 C4 114.4(3) . . . . ? C14 Mo1 C3 C4 47.2(4) . . . . ? C2 Mo1 C3 C8 114.9(5) . . . . ? C6 Mo1 C3 C8 -179.9(4) . . . . ? C13 Mo1 C3 C8 123(4) . . . . ? C1 Mo1 C3 C8 143.3(5) . . . . ? C11 Mo1 C3 C8 37.0(5) . . . . ? C4 Mo1 C3 C8 -114.4(5) . . . . ? C15 Mo1 C3 C8 -36.6(5) . . . . ? C12 Mo1 C3 C8 68.3(5) . . . . ? C5 Mo1 C3 C8 -143.1(5) . . . . ? C10 Mo1 C3 C8 0.0(4) . . . . ? C14 Mo1 C3 C8 -67.2(5) . . . . ? C2 C3 C4 C5 1.8(6) . . . . ? C8 C3 C4 C5 -177.9(4) . . . . ? Mo1 C3 C4 C5 56.0(3) . . . . ? C2 C3 C4 Mo1 -54.1(3) . . . . ? C8 C3 C4 Mo1 126.2(4) . . . . ? C2 Mo1 C4 C5 -102.2(3) . . . . ? C6 Mo1 C4 C5 -29.7(2) . . . . ? C13 Mo1 C4 C5 45.2(4) . . . . ? C1 Mo1 C4 C5 -66.1(2) . . . . ? C11 Mo1 C4 C5 179.9(2) . . . . ? C15 Mo1 C4 C5 112.3(2) . . . . ? C12 Mo1 C4 C5 -74(4) . . . . ? C3 Mo1 C4 C5 -132.0(4) . . . . ? C10 Mo1 C4 C5 149.2(2) . . . . ? C14 Mo1 C4 C5 75.3(3) . . . . ? C2 Mo1 C4 C3 29.7(3) . . . . ? C6 Mo1 C4 C3 102.2(3) . . . . ? C13 Mo1 C4 C3 177.1(3) . . . . ? C1 Mo1 C4 C3 65.8(3) . . . . ? C11 Mo1 C4 C3 -48.1(4) . . . . ? C15 Mo1 C4 C3 -115.8(3) . . . . ? C12 Mo1 C4 C3 58(4) . . . . ? C5 Mo1 C4 C3 132.0(4) . . . . ? C10 Mo1 C4 C3 -78.8(3) . . . . ? C14 Mo1 C4 C3 -152.7(3) . . . . ? C3 C4 C5 C6 -1.3(6) . . . . ? Mo1 C4 C5 C6 54.7(3) . . . . ? C3 C4 C5 C7 178.9(4) . . . . ? Mo1 C4 C5 C7 -125.1(4) . . . . ? C3 C4 C5 Mo1 -56.0(3) . . . . ? C2 Mo1 C5 C4 65.7(2) . . . . ? C6 Mo1 C5 C4 130.9(3) . . . . ? C13 Mo1 C5 C4 -153.1(2) . . . . ? C1 Mo1 C5 C4 102.2(3) . . . . ? C11 Mo1 C5 C4 -171(100) . . . . ? C15 Mo1 C5 C4 -80.7(3) . . . . ? C12 Mo1 C5 C4 176.8(2) . . . . ? C3 Mo1 C5 C4 29.1(2) . . . . ? C10 Mo1 C5 C4 -51.4(3) . . . . ? C14 Mo1 C5 C4 -117.0(2) . . . . ? C2 Mo1 C5 C6 -65.3(2) . . . . ? C13 Mo1 C5 C6 76.0(3) . . . . ? C1 Mo1 C5 C6 -28.8(2) . . . . ? C11 Mo1 C5 C6 58(24) . . . . ? C4 Mo1 C5 C6 -130.9(3) . . . . ? C15 Mo1 C5 C6 148.4(2) . . . . ? C12 Mo1 C5 C6 45.9(3) . . . . ? C3 Mo1 C5 C6 -101.9(3) . . . . ? C10 Mo1 C5 C6 177.7(2) . . . . ? C14 Mo1 C5 C6 112.1(2) . . . . ? C2 Mo1 C5 C7 -178.9(4) . . . . ? C6 Mo1 C5 C7 -113.7(5) . . . . ? C13 Mo1 C5 C7 -37.7(4) . . . . ? C1 Mo1 C5 C7 -142.4(4) . . . . ? C11 Mo1 C5 C7 -55(24) . . . . ? C4 Mo1 C5 C7 115.4(5) . . . . ? C15 Mo1 C5 C7 34.7(4) . . . . ? C12 Mo1 C5 C7 -67.8(5) . . . . ? C3 Mo1 C5 C7 144.5(4) . . . . ? C10 Mo1 C5 C7 64.1(5) . . . . ? C14 Mo1 C5 C7 -1.6(4) . . . . ? C2 C1 C6 C5 0.0(6) . . . . ? C9 C1 C6 C5 179.6(4) . . . . ? Mo1 C1 C6 C5 -55.6(3) . . . . ? C2 C1 C6 Mo1 55.7(3) . . . . ? C9 C1 C6 Mo1 -124.8(4) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C7 C5 C6 C1 -179.9(4) . . . . ? Mo1 C5 C6 C1 55.4(3) . . . . ? C4 C5 C6 Mo1 -55.0(3) . . . . ? C7 C5 C6 Mo1 124.7(4) . . . . ? C2 Mo1 C6 C1 -30.0(2) . . . . ? C13 Mo1 C6 C1 111.7(2) . . . . ? C11 Mo1 C6 C1 48.1(4) . . . . ? C4 Mo1 C6 C1 -103.1(3) . . . . ? C15 Mo1 C6 C1 175.5(2) . . . . ? C12 Mo1 C6 C1 75.4(3) . . . . ? C5 Mo1 C6 C1 -132.4(4) . . . . ? C3 Mo1 C6 C1 -66.6(2) . . . . ? C10 Mo1 C6 C1 119(6) . . . . ? C14 Mo1 C6 C1 147.8(2) . . . . ? C2 Mo1 C6 C5 102.3(3) . . . . ? C13 Mo1 C6 C5 -115.9(2) . . . . ? C1 Mo1 C6 C5 132.4(4) . . . . ? C11 Mo1 C6 C5 -179.5(2) . . . . ? C4 Mo1 C6 C5 29.3(2) . . . . ? C15 Mo1 C6 C5 -52.2(3) . . . . ? C12 Mo1 C6 C5 -152.3(2) . . . . ? C3 Mo1 C6 C5 65.7(2) . . . . ? C10 Mo1 C6 C5 -108(6) . . . . ? C14 Mo1 C6 C5 -79.9(3) . . . . ? C2 Mo1 C10 C15 -153.2(2) . . . . ? C6 Mo1 C10 C15 58(6) . . . . ? C13 Mo1 C10 C15 65.4(2) . . . . ? C1 Mo1 C10 C15 175.4(2) . . . . ? C11 Mo1 C10 C15 130.8(4) . . . . ? C4 Mo1 C10 C15 -79.4(3) . . . . ? C12 Mo1 C10 C15 102.1(3) . . . . ? C5 Mo1 C10 C15 -48.7(3) . . . . ? C3 Mo1 C10 C15 -116.3(2) . . . . ? C14 Mo1 C10 C15 29.0(2) . . . . ? C2 Mo1 C10 C11 76.0(3) . . . . ? C6 Mo1 C10 C11 -73(6) . . . . ? C13 Mo1 C10 C11 -65.4(2) . . . . ? C1 Mo1 C10 C11 44.6(4) . . . . ? C4 Mo1 C10 C11 149.9(2) . . . . ? C15 Mo1 C10 C11 -130.8(4) . . . . ? C12 Mo1 C10 C11 -28.6(2) . . . . ? C5 Mo1 C10 C11 -179.5(2) . . . . ? C3 Mo1 C10 C11 113.0(2) . . . . ? C14 Mo1 C10 C11 -101.8(3) . . . . ? C2 Mo1 C10 C18 -39.5(4) . . . . ? C6 Mo1 C10 C18 171(6) . . . . ? C13 Mo1 C10 C18 179.1(4) . . . . ? C1 Mo1 C10 C18 -70.9(5) . . . . ? C11 Mo1 C10 C18 -115.5(5) . . . . ? C4 Mo1 C10 C18 34.4(4) . . . . ? C15 Mo1 C10 C18 113.7(5) . . . . ? C12 Mo1 C10 C18 -144.2(4) . . . . ? C5 Mo1 C10 C18 65.0(5) . . . . ? C3 Mo1 C10 C18 -2.6(4) . . . . ? C14 Mo1 C10 C18 142.7(4) . . . . ? C15 C10 C11 C12 0.7(6) . . . . ? C18 C10 C11 C12 -179.6(4) . . . . ? Mo1 C10 C11 C12 55.5(3) . . . . ? C15 C10 C11 Mo1 -54.8(3) . . . . ? C18 C10 C11 Mo1 125.0(4) . . . . ? C2 Mo1 C11 C12 110.9(3) . . . . ? C6 Mo1 C11 C12 45.3(4) . . . . ? C13 Mo1 C11 C12 -30.3(2) . . . . ? C1 Mo1 C11 C12 74.4(3) . . . . ? C4 Mo1 C11 C12 176.8(2) . . . . ? C15 Mo1 C11 C12 -102.8(3) . . . . ? C5 Mo1 C11 C12 -12(24) . . . . ? C3 Mo1 C11 C12 147.6(2) . . . . ? C10 Mo1 C11 C12 -132.4(4) . . . . ? C14 Mo1 C11 C12 -66.4(2) . . . . ? C2 Mo1 C11 C10 -116.7(2) . . . . ? C6 Mo1 C11 C10 177.7(2) . . . . ? C13 Mo1 C11 C10 102.1(3) . . . . ? C1 Mo1 C11 C10 -153.3(2) . . . . ? C4 Mo1 C11 C10 -50.9(4) . . . . ? C15 Mo1 C11 C10 29.6(2) . . . . ? C12 Mo1 C11 C10 132.4(4) . . . . ? C5 Mo1 C11 C10 120(24) . . . . ? C3 Mo1 C11 C10 -80.0(3) . . . . ? C14 Mo1 C11 C10 66.0(2) . . . . ? C10 C11 C12 C13 0.1(6) . . . . ? Mo1 C11 C12 C13 55.8(3) . . . . ? C10 C11 C12 C17 179.6(4) . . . . ? Mo1 C11 C12 C17 -124.7(4) . . . . ? C10 C11 C12 Mo1 -55.7(3) . . . . ? C2 Mo1 C12 C11 -80.9(3) . . . . ? C6 Mo1 C12 C11 -152.4(2) . . . . ? C13 Mo1 C12 C11 129.8(4) . . . . ? C1 Mo1 C12 C11 -116.5(3) . . . . ? C4 Mo1 C12 C11 -109(4) . . . . ? C15 Mo1 C12 C11 65.1(2) . . . . ? C5 Mo1 C12 C11 179.9(2) . . . . ? C3 Mo1 C12 C11 -52.9(4) . . . . ? C10 Mo1 C12 C11 28.7(2) . . . . ? C14 Mo1 C12 C11 101.5(3) . . . . ? C2 Mo1 C12 C13 149.3(2) . . . . ? C6 Mo1 C12 C13 77.9(3) . . . . ? C1 Mo1 C12 C13 113.7(3) . . . . ? C11 Mo1 C12 C13 -129.8(4) . . . . ? C4 Mo1 C12 C13 121(4) . . . . ? C15 Mo1 C12 C13 -64.7(2) . . . . ? C5 Mo1 C12 C13 50.1(4) . . . . ? C3 Mo1 C12 C13 177.3(3) . . . . ? C10 Mo1 C12 C13 -101.0(3) . . . . ? C14 Mo1 C12 C13 -28.3(2) . . . . ? C2 Mo1 C12 C17 34.7(4) . . . . ? C6 Mo1 C12 C17 -36.8(4) . . . . ? C13 Mo1 C12 C17 -114.7(5) . . . . ? C1 Mo1 C12 C17 -1.0(4) . . . . ? C11 Mo1 C12 C17 115.6(5) . . . . ? C4 Mo1 C12 C17 7(5) . . . . ? C15 Mo1 C12 C17 -179.4(4) . . . . ? C5 Mo1 C12 C17 -64.6(5) . . . . ? C3 Mo1 C12 C17 62.6(5) . . . . ? C10 Mo1 C12 C17 144.3(4) . . . . ? C14 Mo1 C12 C17 -143.0(4) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? C17 C12 C13 C14 -179.6(4) . . . . ? Mo1 C12 C13 C14 56.0(3) . . . . ? C11 C12 C13 Mo1 -56.0(3) . . . . ? C17 C12 C13 Mo1 124.4(4) . . . . ? C2 Mo1 C13 C14 178.0(3) . . . . ? C6 Mo1 C13 C14 113.5(2) . . . . ? C1 Mo1 C13 C14 150.2(2) . . . . ? C11 Mo1 C13 C14 -102.8(3) . . . . ? C4 Mo1 C13 C14 50.0(4) . . . . ? C15 Mo1 C13 C14 -29.8(2) . . . . ? C12 Mo1 C13 C14 -132.9(4) . . . . ? C5 Mo1 C13 C14 77.3(3) . . . . ? C3 Mo1 C13 C14 170(4) . . . . ? C10 Mo1 C13 C14 -66.3(2) . . . . ? C2 Mo1 C13 C12 -49.1(4) . . . . ? C6 Mo1 C13 C12 -113.6(2) . . . . ? C1 Mo1 C13 C12 -76.9(3) . . . . ? C11 Mo1 C13 C12 30.1(2) . . . . ? C4 Mo1 C13 C12 -177.1(3) . . . . ? C15 Mo1 C13 C12 103.0(3) . . . . ? C5 Mo1 C13 C12 -149.8(2) . . . . ? C3 Mo1 C13 C12 -57(5) . . . . ? C10 Mo1 C13 C12 66.6(2) . . . . ? C14 Mo1 C13 C12 132.9(4) . . . . ? C12 C13 C14 C15 -0.8(6) . . . . ? Mo1 C13 C14 C15 54.9(3) . . . . ? C12 C13 C14 C16 179.4(4) . . . . ? Mo1 C13 C14 C16 -125.0(4) . . . . ? C12 C13 C14 Mo1 -55.6(3) . . . . ? C2 Mo1 C14 C13 -28(3) . . . . ? C6 Mo1 C14 C13 -77.9(3) . . . . ? C1 Mo1 C14 C13 -47.3(3) . . . . ? C11 Mo1 C14 C13 64.9(3) . . . . ? C4 Mo1 C14 C13 -150.4(2) . . . . ? C15 Mo1 C14 C13 130.4(4) . . . . ? C12 Mo1 C14 C13 28.5(2) . . . . ? C5 Mo1 C14 C13 -114.8(3) . . . . ? C3 Mo1 C14 C13 -179.4(3) . . . . ? C10 Mo1 C14 C13 101.4(3) . . . . ? C2 Mo1 C14 C15 -159(3) . . . . ? C6 Mo1 C14 C15 151.7(2) . . . . ? C13 Mo1 C14 C15 -130.4(4) . . . . ? C1 Mo1 C14 C15 -177.7(2) . . . . ? C11 Mo1 C14 C15 -65.5(2) . . . . ? C4 Mo1 C14 C15 79.2(3) . . . . ? C12 Mo1 C14 C15 -101.9(3) . . . . ? C5 Mo1 C14 C15 114.8(2) . . . . ? C3 Mo1 C14 C15 50.2(4) . . . . ? C10 Mo1 C14 C15 -29.0(2) . . . . ? C2 Mo1 C14 C16 86(3) . . . . ? C6 Mo1 C14 C16 36.4(4) . . . . ? C13 Mo1 C14 C16 114.3(5) . . . . ? C1 Mo1 C14 C16 67.0(5) . . . . ? C11 Mo1 C14 C16 179.2(4) . . . . ? C4 Mo1 C14 C16 -36.1(4) . . . . ? C15 Mo1 C14 C16 -115.3(5) . . . . ? C12 Mo1 C14 C16 142.8(4) . . . . ? C5 Mo1 C14 C16 -0.5(4) . . . . ? C3 Mo1 C14 C16 -65.1(5) . . . . ? C10 Mo1 C14 C16 -144.3(4) . . . . ? C11 C10 C15 C14 -1.5(6) . . . . ? C18 C10 C15 C14 178.7(4) . . . . ? Mo1 C10 C15 C14 -56.2(3) . . . . ? C11 C10 C15 Mo1 54.7(3) . . . . ? C18 C10 C15 Mo1 -125.0(4) . . . . ? C13 C14 C15 C10 1.5(6) . . . . ? C16 C14 C15 C10 -178.6(4) . . . . ? Mo1 C14 C15 C10 56.2(3) . . . . ? C13 C14 C15 Mo1 -54.7(3) . . . . ? C16 C14 C15 Mo1 125.1(4) . . . . ? C2 Mo1 C15 C10 46.5(4) . . . . ? C6 Mo1 C15 C10 -178.0(2) . . . . ? C13 Mo1 C15 C10 -102.1(3) . . . . ? C1 Mo1 C15 C10 -101(3) . . . . ? C11 Mo1 C15 C10 -29.6(2) . . . . ? C4 Mo1 C15 C10 114.0(2) . . . . ? C12 Mo1 C15 C10 -65.8(2) . . . . ? C5 Mo1 C15 C10 150.8(2) . . . . ? C3 Mo1 C15 C10 77.2(3) . . . . ? C14 Mo1 C15 C10 -131.8(3) . . . . ? C2 Mo1 C15 C14 178.3(2) . . . . ? C6 Mo1 C15 C14 -46.2(3) . . . . ? C13 Mo1 C15 C14 29.7(2) . . . . ? C1 Mo1 C15 C14 31(3) . . . . ? C11 Mo1 C15 C14 102.2(3) . . . . ? C4 Mo1 C15 C14 -114.2(2) . . . . ? C12 Mo1 C15 C14 66.0(2) . . . . ? C5 Mo1 C15 C14 -77.4(3) . . . . ? C3 Mo1 C15 C14 -151.0(2) . . . . ? C10 Mo1 C15 C14 131.8(3) . . . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .837 _refine_diff_density_min -.687 _refine_diff_density_rms .090